GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o f PFO Ai n Groundwate rSample

s fro m Decatur, A L June/July201 0 

# 3 M

GLP10-01-01

. Interi m Repor t 07 : Analysi s o f PFO Ai n Groundwate rSample s Collecte d a t th e Forme rSludg e Incorporatio n Are a (FSIA ) locate d i n Decatur

. A L i n June/Jul y201 0
Stud yTitl e Analysi s o f Perfluorooctanoi cAci d (PFOA ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Progra m
Dat a Requiremen t EPATSC AGoo d Laborator yPractic e Standard s 4 0 CF R Par t 79 2 Stud yDirecto r Jaisimh a Kesar i P.E. , DE E Westo n Solutions , Inc

. 140 0 Westo n Way Westchester , PA1938 0 Phone : 610-701-376 1 Auttio r Susa n Wol f 3 M Environmenta l Laborator y Interi m Repor t Completio n Dat e

Dat e o f signin g Performin g Laborator y 3 M Environmenta l Healt h an d Safet yOperation s Environmenta l Laborator

y 3 M Center , BId g 260-05-N-1 7 Maplewood , M N 55144 Projec t Identificatio n GLP10-01-01-07 Tota l Numbe ro f Page s

60

Th e testin g reporte d herei n mee t th e requirement

s of iSO/iE C 17025-200 5 "Genera l Requirement

s fo rth e Competenc

e o f Testin g an d Caiibratio n Laboratories" , i n accordanc e wit h th e A21 ACertificate #2052.01

. Testin g that complie s wit h thi s Intemationa i Standar d als o operat e i n accordanc

e wit h IS O 9001:2000

. Certificat e #2052.0 1

Page 1 o f 60GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFOAi n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

Thi s pag e has bee n reserve d fo rspecifi ccountr yrequirements

.

Pag e 2 o f6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o f PFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0



### GL P COMPLIANC E STATEMEN T Repor t Title : GLP10-01-01 , Interi m Repor t 07

. Analysi s o

fPFO Ai n Groundwate rSample s Collecte d a t th e Forme rSludg e Incorporatio n Are a (FSIA ) a t Decatur , A L i n June/Jul y201 0 Study : Analysi s of Perfluorooctanoi cAci d (PFOA ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Program

. Thi s analytica l phas e wa s conducte d i n compliance wit h Toxi cSubstance s Contro l Ac t (TSCA ) Goo d Laborator yPractice (GLP ) Standards , 4 0 CF R 792 , wit h th e exception s liste d below :

• Thes e are environmenta l sample s where there i s n o specifi ctest substance , n o specifi ctest syste m an d n o dosin g of a test system
. • Th e reference substance s hav e no t bee n characterize d unde rth e GLP s an d th e stabilit yunde r storag e condition s a

t th e test sit e hav

e no t bee n determine d unde rGLPs

.

Gar yHohfenstein , Sponso rRepresentative Date 

# QMAC / Jaisimh a Kesari , P.E. , DEE , Stud yDirecto r' Dat e

Pag e 3 o f6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFOAI n Groundwate rSample s fro m Decatur , A L June/Jul y201 0



### QUALIT YASSURANC E STATEMEN T Repor t Title : GLP10-01-01 , Interi m Repor t 07

. Analysi s o

fPFO Ai n Groundwate rSample s Collecte d a t th e Forme rSludg e Incorporatio n Are a (FSIA ) a t Decatur , A L i n June/Jul y201 0 Study : Analysi s of Perfluorooctanoi cAci d (PFOA ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Program

. Thi s repor

t an d th e accompanyin g data were audite d b yth e 3 M Environmenta l Laborator yQualit y Assuranc e Uni t (QAU) , a s indicate d below

. Th e finding s were reporte d t o th e principa l investigato r (P.I.) , laborator

ymanagemen t an d stud ydirector

.

Inspectio n Date s 8/18/10-8/20/1 0 Phas e Data/Interi m Repor

t Dat e Reporte d t o

Testin g Facilit y Managemen t 9/10/1 0 Stud yDirecto r 9/10/1 0



## '^' A O-^ O QA U RepresOTitativ

e Date

Pag e 4 o f6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0



### TABL E O F CONTENT S GL P Complianc e statemen t 3 Qualit yAssuranc e Statemen t 4 Tabl e o f Contents 5 List of Table s 6 1 Stud yInfomnatio n 8 2 Summar

y9 3 Introductio n 1 0 4 Test s Contro l Substance s 1 1 5 Reference Substance s 1 1 6 Test Syste m 1 2 7 Metho d Summar

y1 2 7. 1 Method s 1 2 7. 2 Sampl e Collectio n 1 2 7. 3 Sampl e Preparatio n 1 2 7. 4 Analysi s 1 2 8 Analytica l Results 1 4 8. 1 Calibratio n 1 4 8. 2 Syste m Suitabilit y1 4 8. 3 Limi t o

f Quantitatio n (LOQ ) 1 4 8. 4 Continuin g Calibratio n 1 4 8. 5 Blank

s 1 5 8. 6 La b Contro l Spike s (LCSs ) 1 5 8. 7 Analytica l Metho d Uncertaint y1 7 8. 8 Fiel d Matri xSpike s (FMS ) 1 8

Pag e 5 o f6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o f PFO AI n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

9 Data Summar

yan d Discussio n 1 8 1 0 Conclusio n 2 9 1 1 Data/Sampl e Retentio n 2 9 1 2 Attachment s 2 9 1 3 Signature s 3 0 

### LIS TO F TABLE S Tabl e 1

. Summarize d PFO AResults (FSI AGroundwater , Decatur , AL , June/Jul y2010 ) 1 0 Tabl e 2

. Instalmen t Parameter s 1 3 Tabl e 3

. Liqui d Chromatograph yCondition s 1 3 Tabl e 4

. Mass Transition s 1 3 Tabl e 5

. Limi t of Quantitatio n (LOQ ) 1 4 Tabl e 6

. Laborator

yContro l Spik

e Recover

y1 6 Tabl e 7

. Fiel d Matri xSpik e Level s 1 8 Tabl e 8

. DA L 130 R 0 2 Y1 0 S F 2 0 Tabl e 9

. DA L 130 S 0 2 Y1 0 S F 2 0 Tabl e 10

. DA L 130LQ 2 Y10S F 2 0 Tabl e 11

. DAL131RQ 2 Y10S F 2 1 Tabl e 12

. DA L 131SQ 2 Y10S F 2 1 Tabl e 13

. DAL131LQ 2 Y10S F 2 1 Tabl e 14

. DA L 132 R 0 2 Y1 0 S F 2 2 Tabl e 15

. DA L 132 S 0 2 Y1 0 S F 2 2 Tabl e 16

. DA L 132LQ 2 Y10S F 2 2 Tabl e 17

. DA L 133 R 0 2 Y1 0 S F 2 3 Tabl e 18

. DAL133SQ 2 Y10S F 2 3 Tabl e 19

. DA L 133 L 0 2 Y1 0 S F 2 3 Tabl e 20

. DA L 134 R 0 2 Y1 0 S F 2 4

Pag e 6 o f 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFOAi n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 21

. DAL134SQ 2 Y10S F 2 4 Tabl e 22

. DA L 134 L 0 2 Y1 0 S F 2 4 Tabl e 23

. DA L 135R0 2 Y10S F 2 5 Tabl e 24

. DA L 135S0 2 Y10S F 2 5 Tabl e 25

. DA L 135 L 0 2 Y1 0 S F 2 5 Tabl e 26

. DA L 136 S 0 2 Y1 0 S F 2 6 Table27

. DAL136LQ2Y10S F 2 6 Tabl e 28

. DA L 137 S 0 2 Y1 0 S F 2 6 Tabl e 29

. DA L 137 L 0 2 Y1 0 S F 2 7 Tabl e 30

. DA L 138 S 0 2 Y1 0 S F 2 7 Tabl e 31

. DA L 138 L 0 2 Y1 0 S F 2 7 Tabl e 32

. Tri p Blan k

2 8 Tabl e 33

. Rinseat e Blank s 2 8

Pag e 7 of 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o f PFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0



### 1 Stud yInformatio n Sponso r 3 M Compan y Sponso rRepresentativ e Gar yHohenstei n 3 M EH S Operation s 3 M Buildin g 224-5W-0 3 Sain t Paul , M N 55144-100 0 Phone:(651)737-357 0 Stud yDirecto r Jaisimh a Kesari , P.E. , DE E Westo n Solutions , Inc

. Westchester , P

A1938 0 Phone:(610)701-376 1 Fax:(610)701-740 1 j.kesari@westonsolutions.co m Stud yLocatio n Testin g Facilit y 3 M EH S Operation s 3 M Environmenta l Laborator y Buildin g 260-5N-1 7 Maplewood , M N 5510 6 Stud yPersonne l Willia m K

. Reagen , Ph.D. , 3 M Laborator yManage r Clesto n Lange , Ph.D. , Principa l Analytica l Investigator

. (clanqe(5),mmm.com) : phon e (651)-733-986 0 Susa n Wolf , 3 M Analyst Jonatha n Steege ; Analys t Stud yDate s Stud yInitiation : Marc h 8 , 201 0 Interi m Repor

t 0 7 Experimenta l Termination : August 12,201 0 Interi m Repor

t Completion : Date o

f Interi m Repor

t Signin g Locatio n o f Arcliive s Al l origina l rawdat a an d th e analytica l repor t have bee n archive d a

t th e 3 M Environmenta l Laborator yaccordin g t o 4 0 CF R Par t 792

. Th e tes t substanc e an d analytica l referenc e standard reserv e sample s ar e archive d a t th e 3 M Environmenta l Laborator yaccordin g t o 4 0 CF R Par t 79 2

Pag e 8 o f 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

2 Summar y Th e 3 M Environmenta l Laborator yreceive d groundwate rsample s fro m well s locate d a t th e Forme r Sludg e Incorporatio n Are a (FSIA ) i n Decatur , AL , representin g twenty-fou rdifferen t samplin g locations

. Atota l of on e hundre d twenty-fou rsampl e bottle s were receive d a t th e 3 M Environmenta l Laborator y fo rperfluorooctanoat e (PFOA ) analysis , an d include d duplicat e groundwate rsample s fro m eac h samplin g location

. Sample s als o include d a t least two fiel d matri xspik e (FMS ) sample s fo reac h location , on e tri p blan k

containin g Milli-0 TM wate ran d appropriat e tri p blan k spikes , an d two equipmen t rinseates. Th e equipmen t rinseate blank s di d no t hav e FM S sample s prepare d fo rdetenninatio n of PFO Arecovery . Th e groundwate rsamples , tri p blan k an d two equipmen t rinseate blank s were receive d fro m Westo n personne l o n Jul y6 , 2010

. Al l ofth e sample s were prepare d an d analyze d fo r PFO Afollowin g 3 M Environmenta l Laborator yMetho d ETS-8-044. 0 an d conducte d unde r3 M projec t GLP-10-01-01-07

. Man yof th e groundwate rsample s require d dilutio n t o attai n PFO Aconcentration s withi n th e rang e of th e curve , i n som e instance s u p t o 10(}-fol d dilutio n were required

. Th e averag e measure d PFO

Aconcentration s ar

e summarize d i n Tabl e 1

. Th e equipmen t rinseates an d th e tri p blan k were belo

wth e lowe rlimi t of quantitatio n (LLOQ ) o f0.24 7 ng/mL , indicatin g adequat e contro l o f sampl e contaminatio n durin g shippin g an d sampl e collections

. Th e PFO Aconcentratio n results fo ral l groundwater

s range d ove rthre e order s ofmagnitud e fro m 0.29 7 ng/m L t o 342 0 ng/mL

. Th e analytica l uncertaint ywa s estimate d a

t 10 0 + 4 1 %

.

Pag e 9 o f 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFOAI n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 1

. Summarize d PFOAResult s (FSI AGroundwater , Decatur , AL , June/Jul y2010 )

Sampl e I D DAL130RQ2Y10S F DAL130SO2Y10S F DAL130LO2Y10S F DAL131RO2Y10S F DAL131SO2Y10S F DAL131LO2Y10S F DAL132RO2Y10S F DAL132SO2Y10S F DAL132LQ2Y10S F DAL133RO2Y10S F DAL133SO2Y10S F DAL133LO2Y10S F DAL134RO2Y10S F DAL134SO2Y10S F DAL134LO2Y10S F DAL135RO2Y10S F DAL135SO2Y10S F DAL135LO2Y10S F DAL136SO2Y10S F DAL136LO2Y10S F DAL137SO2Y10S F DAL137LO2Y10S F DAL138SO2Y10S F DAL138LO2Y10S F Tri p Blan k

(Milli-0 TM Water

) Equipmen t rinseate blank s Avg

. PFO A Concentratio n (ng/mL ) 94 2 16 3 86. 8 288 0 [a ] 26. 3 11 5 30 3 141 0 46 4 [a] 193 43 1 25 4 188 0 7.1 7 [b ] 54 0 [a ] 342 0 [a] 17. 5 20 3 11 9 10 7 0.665 0.29 7 [b ] 187 1.8 0 < 0.24 7 < 0.24 7 Relativ e

Percen t Differenc e 0.53 % 0.55 % 1.0 % 2.3 % 5.3 % 1.5 % 1.7 % 1.8 % 0.65 % 1.6 % 1.0 % 1.7 % 0.053 % 1,6 % 2.8 % 1.1 % 7.1 % 2.0 % 1.5 % 0.84 % 14 % 0.0 % 2.4 % 1.7 % N/ A N/ A N/A ; no t applicabl e [a] Samplin g locatio n di d no t hav e a n appropriat e FM S spike leve l t o sufficientl yevaluat e PFO Arecovery . [b ] Fiel d matri xspike di d no t mee t metho d acceptance criteri a of100 % ±30%

. 3 Introductio n Thi s analytica l stud ywa s conducte d as par t ofth e Phas e 3 Environmenta l Monitorin g an d Assessmen t Progra m fo rth e 3 M facilit

ylocate d i n Decatur , Alabama

. Th e objective ofth e overal l progra m i s t o gai n informatio n regardin g concentration s ofperfluorooctanoat e (PFOA ) i n variou s environmenta l medi a suc h as groundwater , soil s an d sediments that ar e associate d wit h an d nea rth e Decatu rfacility

. Thi s analytica l stud ywa s conducte d t o analyz e groun d wate rsample s collecte d fro m variou s well s locate d a t th e Forme rSludg e incorporatio n Are a (FSAI ) i n Decatur , A L fo rPFO Ai n a n effor

t t o characteriz e regiona l groundwate rconditions

. Th e 3 M Environmenta l Laborator yprepare d sampl e bottle s (25 0 m L high-densit ypolyethylene ) whic h were shippe d t o Decatur , A L Westo n personne l prio rt o fiel d sampling

. Sampl e bottl e sets fo reac h groundwate rsamplin g locatio n include d a fiel d sample , fiel d sampl e duplicate , an d a minimu m o ftwo fiel d spik e samples

. Eac h empt

ycontaine rfo rgroundwate rsampling s wa s mari<e d wit h a "fil l t o here " lin e t o produce a fina l sampl e volum e o f20 0 mL

. Container

s designate d fo rfiel d matri xsample s were

Pag e 1 0 o f6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s ofPFO

AI n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

fortifie d wit h a n appropriat e matri xspik e solutio n containin g PFO Aprio rt o bein g sen t t o th e fiel d fo r sampl e collection

. Se e sectio n 8. 8 o f th e repor t fo rfield matri xspik e levels

. Sample s wer e prepare d an d analyze d accordin g t o th e procedur e define d i n 3 M Environmenta l Laboratorymetho d ETS-8-044. 0 "Detenninatio n o f Perfluorinate d Compound s i n Wate rb yHig h Performanc e Liqui d Chromatography/Mas s SpectrometryDirect Injectio n Analysis"

. Tabl e 1 summarize s th e averag e PFO Aconcentration s fo rth e duplicat e groundwate rsample s collected , th e tri p blank , an d equipmen t rinseate samples

. Table s 8-3 3 summariz e th e individua l sampl e result s an d th e associate d FM S recoveries

. Al l result s fo rth e qualit ycontro l sample s prepare d an d analyze d wit h th e sample s ar e reporte d an d discusse d elsewher e i n thi s report
. 

### 4 Tes t & Contro l Substance s Ther e wa s no t a tes t substanc e o rcontro l substance s i n th e classi csens e o f a GL P study

. Thi s stud y wa s purel yanalytica l i n nature
. 

### 5 Referenc e Substance s
Th e analytica l referenc e substance s use d fo rthi s stud yar e liste d below

.

1 Referenc e Substanc e Chemica l Nam e Chemica l Formul a Identifie r Sourc e Expiratio n Dat e Storag e Condition s Chemica l Lo t Number TC R Number Physica l Descriptio n Purit y PFO A Perfluorooctanoat e C7F15COO H CA S # 335-67- 1 Oakwoo d Product s 09/29/201 2 Froze n 344 0 TCR07-004 1 Powde r 99.5 % PFO A Perfluorooctanoat e C7F15COO
Ammoniu m Sal t CA S # 335-67- 1 3 M 02/27/201 7 Froze n 33 2 TCR-12 3 Whit e Powde r 95 %

Pag e 1 1 o f 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFOAI n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

6 Tes t Syste m There wa s no

t a tes t syste m fo rthi s stud yi n th e classi csens e ofa GL P study

. Thi s studywa s conducte d fo ranalysi s o

f groun d wate rsample s collecte d fro m well s locate d i n Decatur , A L b yWesto n Solutions , Inc

. personnel

. Sample s fo rthi s stud yare "rea l worid " environmenta l samples

. Sampl e Descriptio n Ke yCode

. strin g Numbe r Exampl e 1 2 3

4 5 strin g Descripto r DAL132RQ2Y1 0 SF

O Sampl e Locatio n Wel l I D Wel l Leve l
Samplin g Dat e Sampl e Typ e Exampl e DAL = Decatur , Alabam a Example : 132 R = Residu m shallo wwater-bearin g zon e L = Bedroc k

water-bearin g zin e S = Epikars t middl e water-bearin g zon e 0 2 no - 2n d Quarter , 201 0 0=primarysampl e 1=duplicat e sampl e L S = lo wspik e M S = mi d spik e H S = lilgl i spik e

7 Metho d Summar y 7. 1 Method s Analysi s fo ral l analyte s wa s complete d followin g 3 M Environmenta l Laborator ymetho d ETS-8-044. 0 "Detenninatio n of Perfluorinate d Compound s I n Wate rb yHig h Performance Liqui d Chromatography/Mas s Spectrometr yDirec t Injectio n Analysis"

.

..T M , 

### 7. 2 Sampl e Collectio n Sample s were collecte d i n 25 0 m L Nalgene' " (high-densit ypolyethylene ) bottle s prepare d a t th e 3 M Environmenta l Laboratory

. Sampl e bottle s were returne d t o th e laborator ya t ambien t condition s o n Jul y 6,201 0 Sample s were store d refrigerate d a t th e laborator

yafte rreceipt

. Aset oflaborator yprepare d Tri p Blan k

an d Tri p Blan k

fiel d matri xspike s were sen t wit h th e sampl e collectio n bottles

. 7. 3 Sampl e Preparatio n Sample s were prepare d b yremovin g a n aliquot ofth e wel l mixe d sampl e an d placin g i t i n a n autovia l fo r analysis

. Sample s that require d dilutio n were prepare d b ydilution s 1m L sampl e wit h 9 mL s ofMilli- 0 wate r (dilutio n 1:10)

. Som e samplin g location s were dilute d 1:100 b ydilutin g th e 1:1 0 an d additona l wit h Milli
0 water
. 7. 4 Analysi s Al l stud ysample s an d qualit ycontro l sample s were analyze d fo rPFO Ausin g hig h perfomnanc

e liqui d chromatography

/ tande m mass spectrometr y(HPLC/MS/MS)

. Detaile d instmmen t parameters , th e liqui d chromatograph ygradien t program , an d th e specifi cmass transition s analyze d ar e describe d i n th e

Pag e 1 2 o f6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFO AI n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

ra wdata har

d copie s place d i n th e final data packet , an d ar e briefl ydescribe d belo

wi n Tabl e 2 , Tabl e 3 an d Tabl e 4

. Tabl e 2

. Instrumen t Parameters

. instrumen t Nam e Analytica l iUetho d Foiiowe d Analysi s Dat e Liqui d Chromatograp h Guar d colum n Analytica l colum n Injectio n Volum e Mas s Spectromete r Io n Sourc e Electrod e Polarit y Softwar e ETSOiii e ETS-8-044. 0 7/8/1 0 Agilen t 110 0 Betasi l C1 8 (2. 1 m m X 5 0 mm) , 5 u Betasi l C1 8 (2. 1 m m X 100 mm) , 5 n

2or10n L Applie d Biosystem s AP I 400 0 TurtD O Spra y Turtx) io n electrod e Negativ e Analyst 1.4. 2 ETS iVIaryAn n ETS-8-044. 0 8/12/1 0 Agilen t 1200 Betasi l 01 8 (2. 1 m m X 100 mm) , 5 n Betasi l 01 8 (2. 1 m m X 100 mm) , 5 n

1 0 u L /Applied Biosystem s AP I 500 0 Turb o Spra

y Turb o io n electrod e Negativ e /Analys t 1.4. 2 Tabl e 3

. Liqui d Chiromatograpli yConditions

. ste p Numbe r
0 1 2 3 4 5 Tota l Tim e

(min )
0 1. 0 14. 5 15. 5 16. 5 20. 0 Flo wRat e

(fJJmin ) Percen t A

( 2 m M ammoniu m acetate ) ETS-8-044.0 : Analyze d 7/8/1 0 30 0 30 0 30 0 30 0 30 0 30 0 90. 0 90. 0 10. 0 10. 0 90. 0 90. 0 Percen t B

(Methano O
10. 0 10. 0 90. 0 90. 0 10. 0 10. 0 ETS-8-044.0 ; Analyze d 8/12/1 0 0 1 2 3 4 5 0

2. 0 11. 5 13. 5 13. 6 17. 0 30 0

30 0 30 0 30 0 30 0 30 0 97. 0 97. 0 5. 0 5. 0 97. 0 97. 0 3. 0 3. 0 95. 0 95. 0 3. 0 3, 0 Tabl e 4

. Mas s Transitions

.

Analyt e
PFO A Mas s Transitio n

Q1/Q 3 413/36 9 413/21 9 413/16 9 Dwel l tim e wa s 20 0 o r5 0 mse cfo reac h transition

. Th e individua l transition s wer e summe d t o produce a "tota l io n chromatogram " (TIC) , whic h was use d fo rquantitation

.

Pag e 1 3 o f6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o f PFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

8 Analytica l Result s 8. 1 Calibratio n Sample s were analyze d against a n externa l standar d caiibratio n curve . Calibratio n standard s were prepare d b

yspikin g know n amounts ofth e stoc k solutio n containin g th e targe t analyte s int o a laboratory
Mill i 0 water
. Atota l of fifteen spike d standard s rangin g fro m 0.02 5 ng/m L t o 100 ng/m L (nominal ) were prepared , however , no

t al l curve points were analyze d i n bot h analytica l runs . Lo wand/o rhig h curve points were disable d t o mee t accurac yo rlinearit

ycriteria

. Aquadratic , 1/

xweighted , calibratio n curve o f th e pea k are a counts wa s use d t o fit th e data fo reac h analyte

. Th e dat a were no t force d throug h zer

o durin g th e fitting process . Calculatin g th e standar d concentration s usin g th e pea k are a confinne d accurac yof eac h curve point

. Th e calibratio n curve wa s constnjcte d usin g th e linea risome rofPFO A only

. Since th e sample s were expecte d t o contai n bot h linea ran d branche d isomer s ofPFOS , LC S an d sample s were quantitate d b yprocessin g th e PFO

Alinea ran d branche d isomer s separatel yan d summin g th e calculate d concentration s togethe rt o generat e th e final PFO Aconcentration

. Thi s wa s don e t o hel p minimiz e an ypotentia l analytica l bia s du e t o quantitatin g linea ran d branche d isomer s of PFO Aagainst a predominatel ylinea rreference standar d fo rPFOA

. Eac h curve poin t wa s quantitate d usin g th e overal l calibratio n curve an d reviewe d fo raccuracy . Metho d calibratio n accurac

yrequirements of 100±25 % (100±30 % fo rth e lowest curve point) were me t fo ral l analytes

. Th e correlatio n coefficien t (r ) was greate rtha n 0.99 5 fo rPFOA

. 8. 2 Syste m Suitabilit y Acalibratio n standar

d wa s analyze d fou rtime s a t th e beginnin g ofth e analytica l sequence t o demonstrat e overal l syste m suitability

. Al l analyte s met th e acceptance criteri a ofles s tha n o requa l t o 5 % relative standar

d deviatio n (RSD ) fo rpea k are a an d retentio n tim e criteri a o fles s tha n o requa l t o 2 % RS D wa s met
. 

### 8. 3 Limi t o f Quantitatio n (LOQ ) Th e LO O fo rthi s analysi s i s th e lowest non-zer o calibratio n standar

d i n th e curve that meets linearit y an d accurac

yrequirements an d fo rwhic h th e are a counts are a t least twic e thos e o

fth e appropriat e blanks

. Th e nomina l LOO fo ral l analyte s ca n b e foun d i n Tabl e 5

. Tabl e 5

. Limi t o f Quantitatio n (LOQ)

. Analysi s Dat e 7/8/201 0 8/12/1 0 PFOA

LOQ , ng/m L 0.247 0.029 6 8. 4 Continuin g Calibratio n Durin g th e cours e of eac h analytica l sequence , continuin g calibratio n verificatio n sample s (CCVs ) were analyze d t o confimri that th e instrumen t respons e an d th e initia l calibratio n curve were stil l i n control

. Al l CCVs met metho d criteri a of 100 % ±25 % wit h th e exceptio n ofth e following : 7/8/1 0 analysis : Twenty-on e CCVs were analyze d durin g th e cours e ofth e run . Th e endin g thre e CV s had recoverie s of 74. 1 % , 73. 1 % , an d 71.0%

. Reporte d sample s brackete d b ythes e non-complian t CCV S includ e samplin g locatio n DA L 135 L an d th e DA L 132 L H S sample

. Ametho d deviatio n i s filed wit h th e ra

wdata

.

Pag e 1 4 o f 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFOAi n Groundwate rSample s fro m Decatur , A L June/Jul y201 0



### 8. 5 Blank s Thre e type s of blank

s were prepare d an d analyze d wit h th e samples : metho d blanks , tri p blank s an d equipmen t rinseate blanks

. Metho d blan k results were reviewe d an d use d t o evaluat e metho d performance t o detennin e th e LOO fo reac h analyte

. Tri p blank s reflec t th e shippin g an d sampl e collectio n conditon s th e sampl e bottle s an d sample s experience

. Equipmen t rinseate blank s ar e aqueou s sample s that reflec t th e efficienc

yofequipmen t cleanin g i n th e field betwee n differen t sampl e collection s an d are proof of n o cros s contaminatio n ofsample s fro m th e equipment

. 8. 6 La b Contro l Spike s (LCSs ) Low , mid , an d high-leve l la b contro l spike s were prepare d an d analyze d i n triplicat e wit h eac h preparatio n set
. LCS s were prepare d b yspikin g know n amounts o fth e analyt e into 4 0 m L o flaborator y Mill i 0 water , t o produce th e desire d concentration

. Th e spike d wate rsample s were the n analyze d i n th e sam e manne ras th e samples

. Th e metho d acceptance criteria , averag e ofLC S a t eac h leve l shoul d b e withi n 100 % ±20 % wit h a n RS D <20% , were me t foith e linea rPFO

Alo wan d high-leve l o

f LC S sample s analyze d o n 7/8/10

. Th e mid-leve l LC S analyze d o n 7/8/1 0 had a n averag e recover yo f 123%

. Th e mi d an d high-leve l LC S sample s analyze d o n 8/12/1 0 met metho d acceptance criteria , whil e th e low-leve l LC S ha d a n averag e recover yof122%

. A s th e reference material s use d fo rquantitatio n ofPFO Ai s predominantl ylinear , an d th e PFO Apresen t i n th e wate rsample s are comprise d o f linea ran d branche d isomers , additiona l LC S sample s o flinea r an d branche d PFO

Awere prepare d a

t thre e concentration s t o evaluat e th e potentia l fo ranalytica l bias

. Th e linea ran d branche d LC S a t bot h th e mi d an d hig h level s analyze d o n 7/8/1 0 di d no t mee t metho d acceptance criteri a wit h averag e recoverie s of141 % an d 126% , respectively

. Th e low-leve l linea ran d branche d LC S analyze d o n 7/8/1 0 ha d a n averag e recover yof104%

. Th e low , mid , an d high-leve l linea ran d branche d LC S analyze d o n 8/12/1 0 hav e averag e recoverie s of134% , 134% , an d 127% , respectively

. Base d o n th e recover yofth e linea ran d branche d PFO ALCS , i t i s th e opinio n o

fth e laborator ythat th e recover

ydiscrepenc

yofth e linea ran d branche d isomer s ofPFO Aindicate s a n analytica l bias

. Becaus e of thi s bias , th e metho d uncertaint ywil l b e adjuste d t o 100 % ±41% , base d o n th e recover

yof th e linea ran d branche d LC S wit h th e highest averag e recovery . Th e followin g calculation s were use d t o generat e data i n Tabl e 6 fo rlaborator ycontro l spikes :

, „ „ „ . „ Calculate d Concentratio n . . „„. , LC S Percen t Recover

y= * 100 % Spik e Concentratio n

LCS % RS D = standar d deviatio n LC S replicate s . ^ Q^^ ^ averag e LC S recover

y

Pag e 1 5 o f 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o f PFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 6

. Laborator yContro l Spilt e Recovery

. ETS-8-044. 0 Analyze d 7/8/201 0

La b I D LCS-100707- 1 LCS-100707- 2 LCS-100707- 3 Averag e ±%RS D LCS-100707- 4 LCS-100707- 5 LCS-100707- 6 Averag e ±%RS D LCS-100707- 7 LCS-100707- 8 LCS-100707- 9 Averag e ±%RS D Linea rPFO A Spike d Concentratio n (ng/mL ) 0.49 3 0.49 3 0.49 3 Calculate d

Concentratio n (ng/mL ) 0.54 7 0.53 5 0.57 1 VoRecover y

11 1 10 9 11 6 112 % ±3.3 % 4.9 3 4.9 3 4.9 3 6.1 1

5.9 8 6.0 3 12 4

12 1 12 2 123%±1.1%'' ' 29. 6 29. 6 29. 6 31. 6

30. 7 30. 6 10 7

10 4 10 3 105 % ±1.8 % ETS-8-044. 0 Analyze d 7/8/201 0

La b I D LCS-100707-1 0 EC F LCS-100707-1 1 EC F LCS-100707-1 2 EC F Averag e ±%RS D LCS-100707-1 3 EC F LCS-100707-1 4 EC F LCS-100707-1 5 EC F Averag e ±%RS D LCS-100707-1 6 EC F LCS-100707-1 7 EC F LCS-100707-1 8 EC F Averag e ±%RS D Linea r+ Branche d PFO A Spike d Concentratio n (ng/mL ) 0.49 7 0.49 7 0.49 7 Calculate d

Concentratio n (ng/mL ) 0.53 6 0.51 6 0.50 2 VoRecover y

10 8 10 4 10 1 104 % ±3.3 % 4.9 7 4.9 7 4.9 7 6.9 7

7.0 5 7.0 4 14 0

14 2 14 2 141 % ±0.62% TM 29. 8 29. 8 29. 8 38. 6

37. 2 37. 3 12 9

12 5 12 5 126 % ±2.1%'^ ' (1 ) Laborator

ycontro l sampl e averag e recover ydi d no t mee t metho d acceptance criteri a of 100 % ±20%

.

Pag e 1 6 o f 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 6 continued

. Laborator yContro l Splic e Recovery

. ETS-8-044. 0 Analyze d 8/12/201 0

La b I D LCS-100812- 1 LCS-100812- 2 LCS-100812- 3 Averag e ±%RS D LCS-100812 ^ LCS-100812- 5 LCS-100812- 6 Averag e ±%RS D LCS-100812- 7 LCS-100812- 8 LCS-100812- 9 Averag e ±%RS D Linea rPFO A Spike d Concentratio n (ng/mL ) 0.49 3 0.49 3 0.49 3 Calculate d

Concentratio n (ng/mL ) 0.58 3 0.60 9 0.61 7 VoRecover y

11 8 12 4 12 5 122 % ±2.9%'' ' 4.9 3 4.9 3 4.9 3 5.4 6

5.4 8 5.5 9 11 1

11 1 11 3 112 % ±1.3 % 29. 6 29. 6 29. 6 29. 3

29. 4 29. 6 99. 0

99. 3 10 0 99.4 % ±0.52 % ETS-8-044. 0 Analyze d 8/12/201 0

La b I D LCS-100812-1 0 EC F LCS-100812-1 1 EC F LCS-100812-1 2 EC F Averag e ±%RS D LCS-100812-1 3 EC F LCS-100812-1 4 EC F LCS-100812-1 5 EC F Averag e ±%RS D LCS-100812-1 6 EC F LCS-100812-1 7 EC F LCS-100812-1 8 EC F Averag e ±%RS D Ur n Spike d Concentratio n (ng/mL ) 0.49 7 0.49 7 0.49 7 ia r* Branche d P F

Calculate d Concentratio n (ng/mL ) 0.67 7 0.66 3 0.65 9 O A

VoRecover y 13 6 13 3 13 3 134%±1.4%'' ' 4.9 7 4.9 7 4.9 7 6.6 4

6.6 4 6.6 9 13 4

13 4 13 5 134%±0.43%'' ' 29. 8 29. 8 29. 8 38. 0

38. 8 37. 0 12 8

13 0 12 4 127 % ±2.4%'^ ' (1 ) Laborator

ycontro l sampl e averag e recover ydi d no t mee t metho d acceptance criteri a of100 % ±20%

. 

### 8. 7 Analytica l Metho d Uncertaint y Th e analytica l uncertaint

ywa s detennine d base d o n th e qualit ycontro l dat a generate d wit h th e LC S sample s (Tabl e 6 ) an d wa s use d t o evaluat e metho d accurac yan d precision

. Du e t o th e analytica l hig h bias observe d durin g th e quantitatio n ofth e linea r+ branche d PFO Aagainst a calibratio n curve constmcte d fro m th e analysi s of calibratio n standard s containin g linea rPFO Aonly , a n analytica l uncertaint yo f 41 % i s applie d t o al l sampl e results fo rthi s project

.

Pag e 1 7 o f 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFOAi n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

8. 8 Fiel d Matri xSpike s (FMS ) Low , mi d an d hig h fiel d matri xspike s were collecte d a t eac h samplin g poin t t o verif ythat th e analytica l metho d i s applicabl e t o th e collecte d matrix

. Fiel d matri xspike s were generate d b yaddin g a measure d volum e o f fiel d sampl e t o a containe rspike d b yth e laborator

ywit h th e target analyte s prio rt o shippin g sampl e container

s fo rsampl e collection

. Fiel d matri xspik e recoverie s withi n metho d acceptance criteri a of 100±30 % confim n that "unknown " components i n th e sampl e matri xd o no t significantl yinterfer

e wit h th e extractio n an d analysi s o f th e analyte s ofinterest

. Fiel d matri xspik e concentration s mus

t b e 50 % of th e sampl e concentratio n t o b e considere d a n appropriat e fiel d spike

. Fiel d matri xspike s ar e presente d i n sectio n 9 of thi s report
. Tabl e 7

. Fiel d Matri xSpik e Levels

. Samplin g Locatio n 136R , 137R , 137s , 137L , 138 L
130L , 131L , 132L , 133R , 134S , 134L , 136S'^ * 130R , 130S , 131S , 132R , 132S , 133S , 133L , 135S , 135L''' , 136L , 138S<^' , 138 R 131R , 134R , 135 R
Tri p Blan k Spik e Leve l Lo w Mi d Hig h Lo w Mi d Hig h Lo w Mi d Hig h Lo w Hig h Lo w Mi d Mid-Hig h Hig h PFOA , ng/m L

0.098 5 0.98 5 9.85 0.985 9.85 98. 6 9.85 98. 6 98 6 98. 6 98 6 0.98 5 9.8 5 98. 6 98 6 (1 ) On e of th e spike d bottle s i n thi s samplin g set was overfille d b ymor e tha n 10%

. Th e fiel d matri xspik e tm e valu e ha

s bee n adjuste d accordingly

.

„ .„ „ (Sample Concentrationof FMS-Averag e Concentration: FieldSampl e & FieldSampl

e Dup. ) .„,„„„ , FMS Recover

y = -^ ^ ^-^ * 100% Spik e Concentraton
9 Dat a Summar yan d Discussio n Th e table s belowsummariz e th e sampl e results an d fiel d matri xspike recoverie s fo rth e samplin g location s a s wel l a s th e Tri p Blank s an d rinseate blanks

. Results an d averag e value s ar e rounde d t o thre e significan t figure s accordin g t o EP Aroundin g rules

. Becaus e ofrounding , value s ma yvar yslightl y fro m thos e liste d i n th e ra wdata

. Fiel d matri xspik

e recoverie s meetin g th e metho d acceptance criteri a of±30% , demonstrat e that th e metho d wa s appropriat e fo rth e give n matri xan d thei rrespective quantitative ranges . DA L 137L-Th e mid-leve l FM S di d no t mee t metho d acceptance criteri a wit h a recover yo f137%

. Th e high-leve l FM S di d mee t metho d acceptance criteri a wit h a recover yo f122%

. Th e low-leve l FM S wa s no t appropriat e a s compare d t o th e sampl e concentration

.

Pag e 1 8 o f 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o f PFOAi n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

DA L 134 8 - Th e mid-leve l FM S di d no t mee t metho d acceptance criteri a wit h a recover yof137%

. Th e high-leve l FM S di d meet metho d acceptance criteri a wit h a recover yof101%

. Th e low-leve l FM S wa s no t appropriat e a s compare d t o th e sampl e concentration

. DA L 132L
- Du e t o th e hig h concentratio n ofPFO Adetecte d i n th e sample , thi s samplin g locatio n di d no t have a n appropriat e FM S spik e leve l t o sufficientl yevaluat e PFO Arecovery . DA L 134L
- Du e t o th e hig h concentratio n ofPFO Adetecte d i n th e sample , thi s samplin g locatio n di d no t have a n appropriat e FM S spik e leve l t o sufficientl yevaluat e PFO Arecovery . DA L 131R
- Du e t o th e hig h concentratio n ofPFO Adetecte d i n th e sample , thi s samplin g locatio n di d no t have a n appropriat e FM S spik e leve l t o sufficientl yevaluat e PFO Arecovery . DA L 135R
- Du e t o th e hig h concentratio n ofPFO Adetecte d i n th e sample , thi s samplin g locatio n di d no t have a n appropriat e FM S spik e leve l t o sufficientl yevaluat e PFO Arecovery . Tri p Blani t - Th e low-leve l FM S di d no t meet metho d acceptance criteri a wit h a recover yof135%

. Th e mid-leve l FM S di d no t meet metho d acceptance criteri a wit h a recover yof131%

.

Pag e 1 9 o f6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s ofPFO

Ai n Groundwte rSample s fro m Decatur , A L June/Jul y201 0

Tables

. DA L 130RQ 2 Y1 0 S F

3MLIMSI D GLP10-01-01-07-00 1 GLP10-01-01-07-00 2 GLP10-01-01-07-00 3 GLP10-01-01-07-00 4 GLP10-01-01-07-00 5 Descriptio n DAL130RQ2Y10SF 0 DAL130RQ2Y10SF 1 DAL130RQ2Y10SFL S DAL130RQ2Y10SFM S DAL130RQ2Y10SFH S Averag e Concentratio n (ng/mL ) ±%RP D PFO A Concentratio n (ng/mL ) 93 9 944 94 9 104 0 182 0 VoRecover y

N A N A N C N C 88. 7 94 2 ng/m L ±0.53%'^ ' NA = No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level

. (1 ) Samplin g locatio n di d no t hav e a n appropriate spik

e leve l t o evaluate PFO

Arecovery . Tabl e 9

. DA L 130 8 Q2 Y1 0 S F

3MLIMSI D GLP10-01-01-07-00 6 GLP10-01-01-07-00 7 GLP10-01-01-07-00 8 GLP10-01-01-07-00 9 GLP10-01-01-07-01 0 Descriptio n DAL130SQ2Y10SF 0 DAL130SQ2Y10SF 1 DAL130SQ2Y10SFL S DAL130SQ2Y10SFM S DAL130SQ2Y10SFH S Averag e Concentratio n (ng/mL ) ±VoRP D PFO A Concentratio n (ng/mL ) 16 4 16 3 17 9 27 3 117 0 VoRecovery

N A N A N C 11 1 10 2 16 3 ng/m L ±0.55 % N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. Tabl e 10

. DA L 130 L Q2 Y1 0 S F

3MLIMSI D GLP10-01-01-07-01 1 GLP10-01-01-07-01 2 GLP10-01-01-07-01 3 GLP10-01-01-07-01 4 GLP10-01-01-07-01 5 Descriptio n DAL130LQ2Y10SF 0 DAL130LQ2Y10SF 1 DAL130LQ2Y10SFL S DAL130LQ2Y10SFM S DAL130LQ2Y10S F Averag e Concentratio n (ng/mL ) ±VoRP D PFO A Concentratio n (ng/mL ) 86. 3 87. 2 86. 7 53 5 <^ ' 19 4 VoRecover y

N A N A N C N C 10 9 86. 8 ng/m L ±1.0 % N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. (1 ) Th e M S sampl e concentratio n detecte d wa s no t consisten t wit h spik

e level

. Arecover

ywas no t calculated

.

Pag e 2 0 of 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o f PFOAi n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 11

. DA L 131RQ 2 Y1 0 S F

3MLIMSI D GLP10-01-01-07-01 6 GLP10-01-01-07-01 7 GLP10-01-01-07-01 8 GLP10-01-01-07-01 9 Descriptio n DAL131RQ2Y10SF 0 DAL131RQ2Y10SF 1 DAL131RQ2Y10SFL S DAL131RQ2Y10SFH S Averag e Concentratio n (ng/mL ) ±VoRP D PFO A Concentratio n (ng/mL ) 291 0 285 0 296 0 357 0 VoRecover

y NA NA N C N C 288 0 ng/m L ±2.3 % N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. Tabl e 12

. DA L 131 S Q 2 Y1 0 S F

3MLIMSI D GLP10-01-01-07-02 0 GLP10-01-01-07-02 1 GLP10-01-01-07-02 2 GLP10-01-01-07-02 3 GLP10-01-01-07-02 4 Descriptio n DAL131SQ2Y10SF 0 DAL131SQ2Y10SF 1 DAL131SQ2Y10SFL S DAL131SQ2Y10SFM S DAL131SQ2Y10SFH S Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 27. 0 25. 6 38. 1 149 105 0 VoRecover

y NA NA N C 124 10 4 26. 3 ng/m L ±5.3 % NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. Tabl e 13

. DA L 131LQ 2 Y1 0 S F

3IVIUMSI D GLP10-01-01-07-02 5 GLP10-01-01-07-02 6 GLP10-01-01-07-02 7 GLP10-01-01-07-02 8 GLP10-01-01-07-02 9

Averag e Con e Descriptio n

DAL131LQ2Y10SF 0 DAL131LQ2Y10SF 1 DAL131LQ2Y10SFL S DAL131LQ2Y10SFM S DAL131LQ2Y10SFH S entratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 11 6 11 4 11 8 124 188 11 5 ng/m L VoRecover

y NA NA N C N C 74. 1 ±1.5 % N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level

.

Pag e 2 1 o f 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o f PFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 14

. DA L 132RQ 2 Y1 0 S F

3MUIVISI D GLP10-01-01-07-03 0 GLP10-01-01-07-03 1 GLP10-01-01-07-032 GLP10-01-01-07-03 3 GLP10-01-01-07-034 Descriptio n DAL132RQ2Y10SF 0 DAL132RQ2Y10SF 1 DAL132RQ2Y10SFL S DAL132RQ2Y10SFM S DAL132RQ2Y10SFH S Averag e Concentratio n (ng/mL ) ±VoRP D PFO A Concentratio n (ng/mL ) 30 0 30 5 31 2 40 9 125 0 VoRecover

y NA NA N C N C 96. 1 30 3 ng/m L ±1.7 % NA = No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. Tabl e 15

. DA L 132 S Q 2 Y1 0 S F

3MLIMSI D GLP10-01-01-07-03 5 GLP10-01-01-07-03 6 GLP10-01-01-07-03 7 GLP10-01-01-07-03 8 GLP10-01-01-07-03 9 Descriptio n DAL132SQ2Y10SF 0 DAL132SQ2Y10SF 1 DAL132SQ2Y10SFL S DAL132SQ2Y10SFM S DAL132SQ2Y10SFH S Averag e Concentratio n (ng/mL ) ±VoRP D PFO A Concentratio n (ng/mL ) 1430 140 0 139 0 145 0 225 0 VoRecovery

^ NA NA N C N C 84. 4 141 0 ng/m L ±1.8 % N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level

. Tabl e 16

. DA L 132LQ 2 Y1 0 S F

3MLIMSI D GLP10-01-01-07-04 0 GLP10-01-01-07-04 1 GLP10-01-01-07-042 GLP10-01-01-07-04 3 GLP10-01-01-07-044 Descriptio n DAL132LQ2Y10SF 0 DAL132LQ2Y10SF 1 DAL132LQ2Y10SFL S DAL132LQ2Y10SFM S DAL132LQ2Y10SFH S Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 46 2 46 5 47 4 47 3 57 5 VoRecovery

^ NA NA N C N C N C 46 4 ng/m L ±0.65%^' ^ N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level

. (1 ) Samplin g locatio n di d no t hav e a n appropriate spik

e leve l t o evaluate PFO

Arecovery .

Pag e 2 2 o f 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o f PFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 17

. DA L 133 R Q 2 Y1 0 S F

3IVILIMSI D GLP10-01-01-07-04 5 GLP10-01-01-07-04 6 GLP10-01-01-07-04 7 GLP10-01-01-07-04 8 GLP10-01-01-07-04 9 Descriptio n DAL133RQ2Y10SF 0 DAL133RQ2Y10SF 1 DAL133RQ2Y10SFL S DAL133RQ2Y10SFIVI S DAL133RQ2Y10SFH S Averag e Concentratio n (ng/mL ) ±VoRP D PFO A Concentratio n (ng/mL ) 192 195 18 7 193 27 3 19 3 ng/m L VoRecover

y N A NA N C N C 80. 6 ±16 % NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. Tabl e 18

. DA L 133 S Q 2 Y1 0 S F

3MLIMSI D GLP10-01-01-07-05 0 GLP10-01-01-07-05 1 GLP10-01-01-07-05 2 GLP10-01-01-07-05 3 GLP10-01-01-07-05 4 Descriptio n DAL133SQ2Y10SF 0 DAL133SQ2Y10SF 1 DAL133SQ2Y10SFL S DAL133SQ2Y10SFM S DAL133SQ2Y10SFH S Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 42 9 43 3 44 3 53 6 132 0 VoRecover

y NA NA N C N C 90. 1 43 1 ng/m L ±1.0

% N A= No t /Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. Tabl e 19

. DA L 133LQ 2 Y1 0 S F

3MLIMSI D GLP10-01-01-07-05 5 GLP10-01-01-07-05 6 GLP10-01-01-07-05 7 GLP10-01-01-07-05 8 GLP10-01-01-07-05 9 Descriptio n DAL133LQ2Y10SF 0 DAL133LQ2Y10SF 1 DAL133LQ2Y10SFL S DAL133LQ2Y10SFM S DAL133LQ2Y10SFH S Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 25 2 25 6 26 8 37 2 111 0 25 4 ng/m L VoRecover

y NA NA N C N C 87. 1 ±1.7 % N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

.

Pag e 2 3 o f 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o f PFOAi n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 20

. DA L 134RQ 2 Y1 0 S F

3MLIMSI D GLP10-01-01-07-06 0 GLP10-01-01-07-06 1 GLP10-01-01-07-06 2 GLP10-01-01-07-06 3 Descriptio n DAL134RQ2Y10SF 0 DAL134RQ2Y10SF 1 DAL134RQ2Y10SFL S DAL134RQ2Y10SFH S Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 188 0 1880 1940 268 0 VoRecover

y NA NA N C 80. 5 188 0 ng/m L ±0.053 % N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. Tabl e 21

. DA L 134 S Q 2 Y1 0 S F

SMLIMSI D GLP10-01-01-07-07 0 GLP10-01-01-07-07 1 GLP10-01-01-07-072 GLP10-01-01-07-07 3 GLP10-01-01-07-074 Descriptio n DAL134SQ2Y10SF 0 DAL134SQ2Y10SF 1 DAL134SQ2Y10SFL S DAL134SQ2Y10SFM S DAL134SQ2Y10SFH S Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 7.1 1 7.2 3 8.55 20. 7 107 VoRecover

y NA N A N C 137'^ ' 10 1 7.1 7 ng/m L ±1.6 % N A= No t /Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. (1 ) Fiel d matri xspik

e di d no t meet metho d acceptance criteri a of 100 % ±30%

. Tabl e 22

. DA L 134LQ 2 Y1 0 S F

3IVILIMSI D GLP10-01-01-07-07 5 GLP10-01-01-07-07 6 GLP10-01-01-07-07 7 GLP10-01-01-07-07 8 GLP10-01-01-07-07 9 Descriptio n DAL134LQ2Y10SF 0 DAL134LQ2Y10SF 1 DAL134LQ2Y10SFL S DAL134LQ2Y10SFM S DAL134LQ2Y10SFH S Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 54 7 532 54 7 53 0 59 9 VoRecover

y NA NA N C N C N C 54 0 ng/m L ±2.8%^ ' NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. (1 ) Samplin g locatio n di d no t hav e a n appropriate spik

e leve l t o evaluate PFO

Arecoveiy

.

Pag e 2 4 o f 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o f PFO

Ai n Groundwte rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 23

. DA L 135 R Q2 Y1 0 S F

3 M LIM B I D GLP10-01-01-07-06 4 GLP10-01-01-07-06 5 GLP10-01-01-07-06 6 GLP10-01-01-07-06 7 Descriptio n DAL135RQ2Y10SF 0 DAL135RQ2Y10SF 1 DAL135RQ2Y10SFL S DAL135RQ2Y10SFH S Averag e Concentratio n (ng/mL ) ±VoRP D PFO A Concentratio n (ng/mL ) 340 0 344 0 354 0 410 0 VoRecovery

N A N A N C N C 342 0 ng/m L ±1.1%" > N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. (1 ) Samplin g locatio n di d no t hav e a n appropriate spik

e leve l t o evaluate PFO

Arecovery . Tabl e 24

. DA L 135 S Q2 Y1 0 S F

3IVILIMSI D GLP10-01-01-07-08 0 GLP10-01-01-07-08 1 GLP10-01-01-07-08 2 GLP10-01-01-07-08 3 GLP10-01-01-07-08 4 Descriptio n DAL135SQ2Y10SF 0 DAL135SQ2Y10SF 1 DAL135SQ2Y10SFL S DAL135SQ2Y10SFM S DAL135SQ2Y10SFH S Averag e Concentratio n (ng/mL ) ±VoRP D PFO A Concentratio n (ng/mL ) 16. 9 18. 2 28. 4 NA<^' NA'^ > VoRecovery

N A N A 11 0 NA'^ ' NA'^ ' 17. 5 ng/m L ±7.1 % N A= No t Applicabl e (1 ) Samples wer

e re-analyze d o n 8/12/10

. Spik e leve l was no

t analyze d sin e th e L

S wa s th e mos t appropriate spik

e level

. Tabl e 25

. DA L 135 L Q 2 Y1 0 S F

3MLIMSI D GLP10-01-01-07-08 5 GLP10-01-01-07-08 6 GLP10-01-01-07-08 7 GLP10-01-01-07-08 8 GLP10-01-01-07-08 9 Descriptio n DAL135LQ2Y10SF 0 DAL135LQ2Y10SF 1 DAL135LQ2Y10SFL S DAL135LQ2Y10SFMS'^ ' DAL135LQ2Y10SFH S Averag e Concentratio n (ng/mL ) ±VoRP D PFO A Concentiratio n (ng/mL ) 20 1 20 5 20 8 28 6 111 0 VoRecover y

N A N A N C N C 91. 6 20 3 ng/m L ±2.0 % N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level

. (1 ) Sampl e bottl e wa

s overfille d b

ymor e tha n 10%

. Th e FM S tm e valu e wa s adjuste d accordingly

.

Pag e 2 5 of6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o f PFOAi n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 26

. DA L 136 S Q 2 Y1 0 S F

3MLIIVISI D GLP10-01-01-07-09 0 GLP10-01-01-07-09 1 GLP10-01-01-07-09 2 GLP10-01-01-07-09 3 GLP10-01-01-07-09 4 Descriptio n DAL136SQ2Y10SF 0 DAL136SQ2Y10SF 1 DAL136SQ2Y10SFL S DAL136SQ2Y10SFM S DAL136SQ2Y10SFHS'' ' Averag e Concentratio n (ng/mL ) ±VoRP D PFO A Concentratio n (ng/mL ) 11 8 12 0 11 8 12 6 195 VoRecover

y NA NA N C N C 85. 6 11 9 ng/m L ±1.5 % N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level

. (1 ) Sampl e bottl e was overfille d b ymor e tha n 10%

. Th e FM S tm e valu e wa s adjuste d accordingly

. Tabl e 27

. DA L 136 L Q 2 Y1 0 S F

3MLIIVISI D GLP10-01-01-07-09 5 GLP10-01-01-07-09 6 GLP10-01-01-07-09 7 GLP10-01-01-07-09 8 GLP10-01-01-07-09 9 Descriptio n DAL136LQ2Y10SF 0 DAL136LQ2Y10SF 1 DAL136LQ2Y10SFL S DAL136LQ2Y10SFM S DAL136LQ2Y10SFH S Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 107 108 11 3 20 8 102 0 VoRecover

y NA N A N C 10 2 92. 8 10 7 ng/m L ±0.84 % N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. Tabl e 28

. DA L 137 S Q 2 Y1 0 S F

3MLIMSI D GLP10-01-01-07-10 0 GLP10-01-01-07-10 1 GLP10-01-01-07-10 2 GLP10-01-01-07-10 3 GLP10-01-01-07-10 4 Descriptio n DAL137SQ2Y10SF 0 DAL137SQ2Y10SF 1 DAL137SQ2Y10SFL S DAL137SQ2Y10SFM S DAL137SQ2Y10SFH S Averag e Concentratio n (ng/mL ) ±%RP D PFOA Concentratio n (ng/mL ) 0.65 8 0.672 0.76 6 1.8 4 12. 1 VoRecover

y NA NA N C 12 0 11 6 0.66 5 ng/m L ±14 % N A= No t /\pplicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level

.

Pag e 2 6 o f 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 29

. DA L 137 L Q 2 Y1 0 S F

3MLIMSI D GLP10-01-01-07-10 5 GLP10-01-01-07-10 6 GLP10-01-01-07-10 7 GLP10-01-01-07-10 8 GLP10-01-01-07-10 9 Descriptio n DAL137LQ2Y10SF 0 DAL137LQ2Y10SF 1 DAL137LQ2Y10SFL S DAL137LQ2Y10SFM S DAL137LQ2Y10SFH S Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 0.29 7 0.29 7 0.41 7 1.6 5 12. 1 VoRecover

y N A NA N C 13 7 <^ ' 122 0.29 7 ng/m L ±0.0 % NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level

. (1 ) Fiel d matri xspik

e di d not meet metho d acceptance criteri a of 100 % ±30%

. Tabl e 30

. DA L 138 S Q 2 Y1 0 S F

3MLIMSI D GLP10-01-01-07-11 0 GLP10-01-01-07-11 1 GLP10-01-01-07-11 2 GLP10-01-01-07-11 3 GLP10-01-01-07-11 4

Averag e Con e Descriptio n

DAL138SQ2Y10SF 0 DAL138SQ2Y10SF 1 DAL138SQ2Y10SFLS<^ ' DAL138SQ2Y10SFM S DAL138SQ2Y10SFH S entratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 189 18 4 197 29 1 1080 18 7 ng/m L VoRecover

y NA NA N C 106 90. 1 ±2.4 % N A= No t /Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level

. (1 ) Sampl e bottl e was overfille d b ymor e tha n 10%

. Th e FM S tnj e valu e wa s adjuste d accordingly

. Tabl e 31

. DA L 138 L Q 2 Y1 0 S F

3MLIIVISI D GLP10-01-01-07-11 5 GLP10-01-01-07-11 6 GLP10-01-01-07-11 7 GLP10-01-01-07-11 8 GLP10-01-01-07-11 9 Descriptio n DAL138LQ2Y10SF 0 DAL138LQ2Y10SF 1 DAL138LQ2Y10SFL S DAL138LQ2Y10SFM S DAL138LQ2Y10SFH S Averag e Concentratio n (ng/mL ) ±VoRPD PFOA Concentratio n (ng/mL ) 1.7 8 1.8 2 1.8 8 3.03 13. 1 VoRecover

y NA NA N C 12 5 11 5 1.80 ng/m L ±1.7 % NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level

.

Pag e 2 7 o f 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 32

. Tri p Blan k

3MUIi/ISI D GLP10-01-01-07-12 4 GLP10-01-01-07-12 0 GLP10-01-01-07-12 1 GLP10-01-01-07-12 2 GLP10-01-01-07-12 3 Descriptio n TRI P BLAN K0 TRI P BLAN KL

S TRIPBUANKM S TRI P BLAN KMH S TRI P BLAN KH S PFOA Concentratio n (ng/mL ) <0.24 7 1.3 3 12. 9 11 5 121 0 VoRecover

y NA 135'^ ' 13 1 '^ ' 11 7 123 N A= No t Applicabl e (1 ) Fiel d matri xspik

e di d no t meet metho d acceptance criteri a o f 100 % ±30%

. Tabl e 33

. Rinseat e Blank s

3MLIMSI D GLP10-01-01-07-06 8 GLP10-01-01-07-06 9 Descriptio n DAL137LQ2Y10SFR B DAL131RQ2Y10SFR B PFOA Concentratio n (ng/mL ) <0.24 7 <0.24 7 VoRecover y NA NA N A= No t /Applicabl e

Pag e 2 8 o f 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFOAi n Groundwate rSample s fro m Decatur , A L June/Jul y201 0



### 1 0 Conclusio n Laborator ycontro l spike s an d fiel d matri xspike s were use d t o determin e th e analytica l metho d accurac yan d precisio n fo rPFOA

. Analysi s wa s successfull ycomplete d followin g 3 M Environmenta l Laborator ymetho d ETS-8-044. 0 describe d herein

. 1 1 Data/Sampl e Retentio n Al l remainin g sample s an d associate d projec t data (hardcopyan d elecrtronic ) wil l b e archive d accordin g t o 3 M Environmenta l Laborator ystandar d operatin g procedures

. 

### 1 2 Attachment s Attachmen t A : Protoco l Amendmen t 0 7 (Genera l Projec t Outline ) Attachmen t B : Representative Chromatogram s an d Calibratio n Curve s Attachmen t C : Analytica l Metho d Attachmen t D : Metho d Deviatio n

Pag e 2 9 o f 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0



### 1 3 Signature s

Date Clesto n Lange , Ph.D. , 3 M Principa l Analytica l Investigato r 

## / y J^^<^Poy o Willia m K

. Reagen , Ph.D. , 3 M Environmenta l Laborator yManage rDate



# I d Gar yHohertstdh , 3 M Sponso rRepresentative 

# 4Whl, i Date

' / Date Jaisimh a Kesari , Stud yDirecto r

Pag e 3 0 o f 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFO Ai n Groundwate rSample s fro m Decatur , A L Attachmen t AJune/Jul y2010,

. , „ , , ^ , „^ ^ „ ^ „ ^ Analytica l Protocol : GLP10-01-0 1

Amendmen t 0 7



### Stud yTitl e Analysi s o f Perfluorooctanoi cAci d (PFOA ) I n Groundwater , Soi l an d Sedimen t fo rth e

3 M Decatu rPhas e 3 Site-Relate d Monitorin g Progra m

PROTOCO L AMENDMEN TNO

. 0 7

Amendmen t Date : Jun e 16 , 201 0
Performin g Laborator y 3 M Environmental , Health , an d SafetyOperation s

3 M Environmenta l Laborator y Buildin g 260-5N-1 7 Maplewood , M N 55144-100 0

Laborator yProjec t Identificatio n

GLP10-01-0 1
Samplin g Even t Forme rSludg e Incorporatio n Are a (FSIA ) Groundwate r

Pag e 1 o f8 Pag e 3 1 o f6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFOAi n Groundwate rSample s fro m Decatur , A L Attachmen t AJune/Jul v2010^

. , „ ^

. ^ , r,^/ , ^ > o > Analytica l Protocol : GLP10-01-0 1

Amendmen t 0 7 

### Thi s amendmen t modifie s th e followin g portio n o fprotocol : "Analysi s o f Perfluorooctanoi cAci d (PFOA ) i n Groundwater , Soi l an d Sedimen t fo rth e

3 M Decatu rPhas e 3 Site-Relate d Monitorin g Program "

PROTOCO L RBADS : Sectio n 9.2. 1 : Astabl e isotope-labele d interna l standard , [(1,2,3,4,5,6,7,8-"C8)-PFOA] wil l b e adde d t o eac h sample , LMS , LCS , procedura l blan k an d calibratio n standard fo raidin g quantitatio n ofPFO Aan d th e surrc^ate

. Astabl e isotope-labele d sumagat e [(1,2,3,4-"C4)-PFOA] wil l als o b e adde d a t a fixe d leve l t o eac h sample , LMS , LCS , procedura l blank , an d a t variabl e know n concentration s i n calibratio n standards , an d quantifie d t o determin e surrogat e recoveries

.

AMEN D r o KBAD : Astabl e isotope-labele d intema l standard

. [{1,2,3,4.5,6,7.8-"C8)4'FOA] mayb e adde d t o eac h sample , LMS , LCS , procedura l blan k

an d calibratio n standar

d fo raidin g quantitatio n ofPFO Aan d th e surrogate
. Astabl e isotope-labele d sun-ogate [{1,2,3,4-^^C4)-PFOA ] ma yals o b e adde d a

t a fixe d leve l t o eac h sample , LMS

. LCS , procedura l blank , an d at variabl e know n concentration s i n calibratio n standards , an d quantifie d t o detennin e surrogat e recoveries

. Th e us e of intema l standard s an d sunnogate s are onl yappropriat e fo rthos e samplin g location s wit h PFO

Acoricenlraflon s i n th e lowpp b range . Prio rt o eac h samplin g event , i fpreviousl yobtaine d PFO Adat a i s availabl e fo rth e samplin g points cifinteres t ttie data wil l b e reviewe d t o determin e i fth e us e of intema l standard s an d surrogate s i s appropriat e fo rth e curren t samplin g event
.

PROTOCO L RBADS : N o change s t o th e wordin g o f th e protoco l ar e required

.

AMEN D T O READ : N o change s t o th e wordin g o f th e protoco l are required

. Thi s amendmen t onl yaddresse s an d document s Vtx e additio n o f th e Genera l Project Outiin e (GPO ) fo rth e coilectid n an d analysi s o fgroundwate rsample s a t Decatur , AL

. an d conducte d a s part of th e 3 M Decatu rPhas e 3 Progra m fo rPFO A(GLP10-01-01)

. Th e anticipate d sampl e coiiectio n wil l occu raroun d th e timeframe o fJun e 21

. 2010

. Th e groundwate r sample s fo rthi s samplin g even t wil l b e entere d int o th e 3 M Environmenta l Laborator yLIM S a s project GLP10-01-01-0 7 an d reporte d a s interi m report GLP10-01-01-07 , (reflectin g stud yGLP10-01-0 1 an d amendmen t -07).

Reason : Th e reaso n fo rthi s amendmen t i s t o documen t th e Genera l Projeci t Outlin e (GPO ) whic h describe s th e anticipat e groundwate rsampl e collectio n even t t o b e conducte d fo rth e 3 M Decatur , A L facility

. Th e GP O i s fou rpage s i n lengt h an d include d a s attache d t o tiiis amendmen t fonn

.
Pag e 2 o f8 Pag e 3 2 o f 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFOAi n Groundwate rSample s fro m Decatur , A L Attachmen t AJune/Jul v2010^

. , „ ^ , ^

. r,^

^ ^

. ^ > Analytica l Protocol : GLP10-01-0 1

Amendmen t 0 7



### Amendmen t Approva l

Gar yHohenstein , Sponso rRepresentative Date 

# 7 Clesto n C

. Lange , Principa l Analytica l Investigato rDat e

Willia m Reagen , EH S Opjn s Environmenta l La b Managemen t Dat e

Jaisimh a Kesar i P.E. , DEE , Stud yDirecto rDate

Pag e 3 o f8 Pag e 3 3 o f 6 0Attachmen t A GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFOAi n Groundwate rSample s fro m Decatur , A L June/Jul y201 0 Analytica l Protocol : GLP10-01-0 1

Amendmen t 0 7 

### Environmenta l Healt h & SafetyOperations , Environmenta l Laborator y Genera l Projec t Outlin e To : Gar

yHohenstein , 3 M EHS&Opn s From : Susa n Wolf , 3 M EHS&Opns ; Environmenta l La b cc : Willia m Reagen , 3 M EHS&Opns ; Environmenta l La b Cliffto n Jacoby , 3 M EHS&Opns ; Environmenta l La b Ja i Kesari , Westo n Solution s Charle s Young , Westo n Solution s Ti m Frinak , Westo n Solution s Date : Jun e 16,201 0 Subject : Analysi s o f Perfluorooctanoi cAci d (PFOA ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M

Decatu rPhas e 3 Site-Relate d Monitorin g Program ; GL P Interi m Report 0 7 - Fonme rSludg e Incorporatio n Are a (FSIA ) Groundwate r 

### 1 Genera l Projec t Informatio n

Contact s

La b Reques t Numbe r SixDigi t Departmen t Numbe r Projec t Schedule/Tes t Date s 3 M Sponso rRepresentativ e Gar yHohenstei n 3 M EH S Operation s 3 M Buildin g 224-5W-0 3 Sain t Paul , M N 55144-100 0 Phone:(651)737-357 0 aahohensteiniammm.co m 3 M Environmenta l Laborator yManagemen t Willia m K

. Reage n 3IVI EH S Opns , Environmenta l Laborator y 260-5N-1 7 65 1 733-973 9 wkreaaen(a!mmm.cora Principa l Analytica l Investigato r Clesto n Lang e 3 M EH S Opns , Environmenta l Laborator y 260-5N-1 7 65 1 733-986 0 cclanaeOmmm.co m Santpliri g Coordinato r Timoth yFrina k Westo n Solution s Tlmothv.frinak(a!westonsolutions.co m Phone : (334).332^912 3 GLP10-01-01-0 7 Dep t #530711 , Proiect #002267444 9 Samplin g schedule d fo rth e wee k o fJun e 21 , 201 0 Al l verba l an d writte n correspondenc e wil l b e directe d t o Gar yHohenstein

. Pag e 4 o f8 Pag e 3 4 o f6 0Attachmen t A GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0 Analytica l Protocol : GLP10-01-0 1

Amendmen t 0 7 

### 2 Backgroun d Informatio n an d Projec t Objective(s ) Th e 3 M EH S Operation s Laborator y(3 M Environmenta l Lab ) wil l receiv e an d analyz e groundwate r sample s cx)llecte d fro m twenty-seve n groundwate rwell s fo rPerfluorooctanoi cAci d (PFOA ) fro m th e Forme rSludg e Incorporatio n Are a (FSIA)

. Analyse s wil l b e conducte d unde rth e GL P requirement s o f EPATSC AGoo d Laborator yPractic e Standard s 4 0 CF R 792

. Groundwate rsample s fro m Decatur , A L wil l b e collecte d b yWesto n Solution s personne l th e wee k o fJun e 21 , 2010

. Th e 3 M Environmenta l Laborator ywil l prepar e th e sampl e bottle s wit h al l require d spike s t o ensur e tha t result s fo rPFO Aar e o f a know n precisio n an d accuracy . Th e final report wil l b e submitte d t o Gar yHohenstei n an d Ja i Kesar i upo n completio n unde rinteri m repor t GLP10-01-01-07

. 

### 3 Projec t Schedul e Sampl e collectio n bottle s wil l b e prepare d b y3 M Environmenta l Laborator yfo rsamplin g Ui e wee k

ofJun e 21 , 2010

. Sampl e bottle s wil l b e shippe d i n cooler s overnigh t t o 3 M Decatu rfo rarriva l o n Friday , Jun e 18 , 2010

. Sampl e bottle s shoul d b e store d refrigerate d on-sit e unti l sampl e collection

. Marti n Smit h \

Westo n Traile r 3 M Decatu rPlan t 140 0 Stat e Docks Roa d Decatur , Alabam a 3560 1 

### 4 Tes t Parameter s Th e targete d limi t of quantitatio n wil l b e 0.02 5 ng/m L (ppb ) fo rPFOA

. Atota l o f twenty-seve n samplin g location s have bee n specified

. Fo reac h samplin g location , a sample , sampl e duplicat e an d a minimu m of tw o field matri xspike s wil l b e collected

. Tabl e 1 indicate s tiie wel l I D an d correspondin g fiel d spike levels

. Th e "fil l t o here " lin e o n eac h 25 0 m L Nalgen e bottl e wil l b e 20 0 mL

. Thre e set s of tri p blank

s consistin g o f reagent-grad e water , a low-leve l tilp blan k spike , mid-leve l fiel d spike , mid-hig h fiel d spike , an d a high-leve l tri p blan k spik e wil l b e prepare d at th e 3 M Environmenta l Laborator yan d sen t t o th e samplin g locatio n wit h th e othe rbottles

. Two additiona l bottle s wil l b e prepare d t o b e use d fo rth e preparatio n o f th e equipmen t rinseate blanks

. Atota l o f 145 sampl e bottle s wil l b e prepared

. Tabl e 1

. Sampiin g Location s an d Fiel d Matri xSpik e levels

. Wel l No

. 136R , 137R , 137S , 137L , 138 L 130L , 131L , 132L , 133R , 134S , 134L , 136 S 130R , 130S

. 131S

. 132R , 132S , 133S , 133L , 135S

. 135L

. 136L

. 138S , 138 R 131R , 134R , 135 R TripBlankSe t 1,2 , and 3 Sampl e Leve l Lo w Mi d Hifl h Lo w Mi d Hig h Lo w Mi d Hig h Low HIp h Low Mi d Mid-Hig h Hig h Spik e Cone

. (ng/mL ) 0. 1 1. 0 1 0 1 1 0 10 0 1 0 10 0 100 0 10 0 100 0 1 1 0 10 0 100 0
Pag e 5 of8 Pag e 35 o f 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o f PFO Ai n Groundwate rSample s fro m Decatur , A L Attachmen t AJune/Jul y201 0 Analytica l Protocol : GLP10-01-0 1

Amendmen t 0 7

5 Tesi t Method s Sample s wil l b e prepare d an d analyze d b yLC/MS/M S followin g ETS-8-044. 0 "Detenninatio n o fPerfluorinate d Compound s I n Wate rbyHig h Performance Liqui d Chromatography/Mas s Spectrometi yDirec t Injectio n Analysis"

. Th e dat a qualit yobjective s fo rttiese studie s are quantitative results fo rth e targe t analyte s witf i a n analytica l accurac

yof 100+30%

. Fiel d matri xspike s no t yieldin g recoverie s withi n 100±30 % wil l b e addresse d i n th e repor

t an d th e fina l accurac

ystatemen t ma

yb e adjuste d accordingly

. Alternately , sample s ma yb e analyze d byETS 8-154. 3 "Determinatio n ofPerfluorinate d Acids , Alcohols , Amides , an d Sulfonate s I n Wate rB ySoli d Phas e Extractio n an d Hig h Performance Liqui d Chromatography/Mas s Specti-omety

. MeUiod ETS-8-15 4 has bee n validate d fo rPFO Aan d PFO S only ; however , specifi cqualitycontro l sample s analyze d wit h th e sample s wil l b e use d t o detennin e overal l metho d precisio n an d accxinacy

. 6 Reportin g Requirement s Fo reac h samplin g location , th e repor t wil l contai n th e resufte forth e sample , sampl e duplicate , an d field matii x spikes

. Tri p blan k

an d tri p blan k

spike s wil l b e reporte d fo rfrie samplin g even t a s wil l an yequipment/rinseat e blank s prepare d i n th e field. Laborator ycontro l spike s ofreagen t wate rprepare d at th e time o fsampl e preparatio n wil l als o b e reporte d an d use d t o evaluat e th e overal l metho d accurac yan d precision

. Metho d blank s of reagen t wate rprepare d at th e time o fsampl e preparatio n wil l b e use d t o determin e th e metho d detectio n limit

. Fo rthos e samplin g location s where th e field matii xspike leve l wa s not appropriate , du e t o highe rtha n expecte d analyt e concentirations , a laborator ymatri xspike ma

yb e prepare d an d wil l ti e include d i n th e final report 

## 7 Emai l Correspondenc e Attachmen t A : Samplin g Bottl e Request

Pag e 6 o f8 Pag e 3 6 o f 6 0Attachmen t A GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFOAi n Groundwate rSample s fro m Decatur , A L June/Jul y201 0 Analytica l Protocol : GLP10-01-0 1

Amendmen t 0 7

Projec t Duration : 2 1 Jun e throug h 2 Jul y201 0 Dat e Required : 18-Jun-l O
Shi p Container s to : Westo n Solutions , Inc

. Fiel d Offic e 3 M Decatu rPlan t 140 0 Stat e Dock s Roa d Decatur , A i 3560 1 

### 256-552-618 9 Attn : Marti n Smit h

Sampl e Medi a Groundwate r Sampl e Containe rRequirement s Sample s 2 7 Duplicat e

Sample s n a Rinsat e Blan k

Sets 2 Tri p Blan k

Sets Se e Not e 1
Not e 1 : On e tri p blan k

wil l b e require d fo reac h shippin g containe rreturne d t o th e laboratory

. I t shoul d b e note d tha t ic e wil l b e require d fo rshipment s o fsoi l / sedimen t sample s whic h rrtayresul t i n a n increas e i n th e numbe ro f shippin g container s (an d tri p blanks ) required

. Not e 2 : Rinsat e Blan k

Sets shoul d b e accompanie d wit h a n appropriat e volum e o f wate rt o accomplis h th e sampling

. Th e volum e shoul d accoun t fo rspillag e durin g th e rinsin g process . Not e 3 : Pleas e not e tha t an ybottl e set s no t use d du e t o uniqu e fiel d condition s wil l b e isolate d an d returne d t o th e laborator ylabele d fo rdisposal

.

Pag e 7 o f 8 Pag e 3 7 of6 0Attachmen t A GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFOAi n Groundwate rSample s fro m Decatur , A L June/JulY201 0 Analytica l Protocol : GLP10-01-0 1

Amendmen t 0 7

Well s Include d i n Thi s Samplin g Event : Wel l No . 130R 130 S 130 L 131 R 1 3 I S 131 L 132 R 132 S 132 L 133 R 133 S 133 L 134 R 134 S 134 L 13S R 135 S 135 L 136 R 136 $ 136 L 137 R 137 S i37 L 138 R 138 S 138 L

Pag e 8 o f 8 Pag e 3 8 o f 6 0*011ie : U001104O 2 Attachmen t B GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o f PFO AI n Groundwate rSample s fro m Decatur , A L June/Jul y201 0
o100708 a linear.rd b {PFOA_TIC) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -6.42e+00 3 x'^ 2 + 1.16e+00 6 x+ 2e+00 5 ( r= 0.9992 )

t n 

### 8

of < O.ZS I 6.0e7

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### • / / / / / / / / / / 

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# -4yV

Printin g Time : 12:05:5 8 P M Printin g Date : Monday , Septembe r 13 , 201 0 Pag e 4 0 o f 6 0 *011ie : U0011040 2

I Sampl e Nama : •o100708a023 - Sampt e ID : "0 3 008-147-1( rFile : "o100708a.wf r Paa k Nanna : •PFOA_T)C " M8ss(o6) : "413.0/369. 1 amu.413.0/168. 9 amu.413.0/218. 8 a I ComfTwrtt : "5. 0 pp b curv « poin t i n Mitti O Water " Annotation: "

V0ee 6 1.06e6 ' 1.048 6 1.02e 6 I.OOe e g.80e 5 9.60e5 ' 9.40e 5 9.20e 5 S.DOeS

e.80e5

- e.60o5 ' e.40« 5 6J?0a5

- 8.00e 5 7.BOe 5 7.60e5

- 7.40e 5 7.20* 5 7.00e5 ' 6.eOe5

- 6.60e 5 6.40e 5 6.20e 5 e.OOe S 5.80e5

- 5.6O0S

5.40e 5 S.20e 5 5.00e 5 4.B0e 5 4.60e 5 4.40e5

- 4.20« 5 4.00e 5 3.80e5

- 3.60e5

- 3.40e 5 3.20e 5 3.OO0 S 2.80e 5 2.60e S Z40«5

- 2.20e 5 2.00e5 ' 1.60e 5 1.60e 5 1.40e 5 1.20e 5 I.OOe S e.00e 4 6.00e 4 4.00e 4 2.00e4

- 0,0 0 0.8 4

A *Dat a work-u p performe d b yST W Pag e 1 o f 6*011ie : U0011040 2 GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o f PFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

I Sarnpl e Name : "01007083030 " Sampl e ID : 'Solven t Blan k (Milli Q Elerrwnt rFile : "oi00708a.wif T Pea k Name : *PFOA_TI C Mass(es]:'413.0/369. 1 aniu,413.0/168.daniu.413.0/218. 8 I Comment:"TN10-0237 " Annotation:' "

ModiCied : R TWindow ; Exfjcte d BT :

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Printin g Time : 12:05:5 8 P M Printin g Date : Monday , Septembe r 13 , 201 0 Pag e 4 2 o f6 0 *011ie : U0011040 2 

# I Sairpt e Name : '01007083039
- Sampl e ID : "LCS-100707-7 ' File : 'ol00708a.wt r Pea k Name : 'PFOA_TI C Mass(e«) : "413.ora69. 1 amu,413.0/168. 9 amu.413.0/218. 8 amu " Commen t "3(^>p b LCS " Annotation ; ~

4.8e 6 4.7e6

- 4.6a 6 Hodifi i R TWin

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- 2.0e 6 1.9e 6 1.8e 6 1-7e 6 1.6a 6 1.5e 6 1.4« 6 V3e 6 1.2e6

- l.le S l,0a 6 e.Oe S 8.0e 5 7.0e 5 6.0e 5 S.Oe S 4.0e 5 3.0e 5 2.0e5

- I.Oe S 0. 0
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# I Sampl e Name : "01007083050 " Sampl e ID : "LCS-100707-14 " File : "o100708a.«M r Pea k Name : "PFOA.TI C Pifas$<es) : "413,0/369. 1 arnu,413.0/168. 9 amu.413.0/218. 8 amu ' Comment : "5pp b LC" s ECF " Anno&tion: "

*Dat a work-u p performe d b yST W Pag e 4 o f 6 Printin g Time : 12:05:5 8 P M Printin g Date : Monday , Septembe r 13 , 201 0 Pag e 4 3 o

f 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFOAi n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

Printin g Time : 12:05:5 8 P M Printin g Date : Monday , Septembe r 13 , 201 0 Pag e 4 4 o f6 0 •Ollie : U0011040 2 

# I Sampt o Name:-olOOTOaaOTB
- Sampt e ID : *G1.P1(W)1^31.07-115 " Fila : "o10070aa.w r Pea k Name:'PFO ATI C Masc<ea):'413.0/369. 1 aiTiu.413.Dn€8.9amu.413.(V218. 8 amu ' Comment'DAL138lQ2Y10SF( rAnnotafion: " Sampl e InJsJ-. ; "I S Simpl e Type ; Unl-.no--ii n Calc'ilate dCone : 1.5 1 ng/m L Acq
. Date : 7/9/201 0 Arq
. Time : i:5i:3 4 P H Wodifisd : R T Window : Exp«cce dR

T U3 hP.^lativ f Int
. Type : Retentio nT Area : Heigfit : Star t Tine : EndTi»e : ye s

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o Manual ne : H. ? ni n 5Sei9 5 cp s U . l mi n U . i min 3.5*5

-

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# I SatTpleName:*o10a708a117 ' Sampl e ID;'GLP1O01431.07.040 ' f He:'o10070ea.wi r Pea k Name:'PFOA_T[ C Mass^es):'413.07369. 1 amu.413.0/168.9amu,413.0/218. 8 amu ' CofT«ient'DAL132LQ2Y10SF 0 (dil1:10 rAnnotation: ~ Sam{;l & Indax : 11 7 Sjn.p l Calc
. Acq
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- 2.7* 6 • 2.6* 6 Z5e 6 2.4* 6 2.3* 6 2.2* 6 2.1* 6 Z0e6

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- 0. 0 *Dat a work-u p performe d b yST W Pag e 6 o f 6GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o f PFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

Printin g Time : 12:07:0 7 P M Printin g Date : Monday , Septembe r 13 , 201 0 Pag e 4 6 o f 6 0 ^Ollie : U0011040 2

• Sampl e Nam*:'0100708*050 ^ SampI * ID : TCS-l00707-14 " File:'o10070aa.Mif r • Pea k Nam*:-PFOA_TIC
- Ma»«(*s):-413.0/369. 1 anw,413.0n68.9amu,413.W218.8«mu
B Comm*n t '5pp b LC S EC P Anrwbtion : ~ Sddipl e Type : Unknow n Calculate dCone : 1.1 1 ng/m L Acq
. Dat« : 7/9/201 0 Acq
. Tirae : 5:03:3 2 A M 1. 2 «odi£ied : Proc
. Algorithm : Nois « P«r!,-a.ita7 « Base
. 3Mb
. Wind c Peak-Split
. Fac t Repor t Larges t

P Min
. Pea k

Heiyh t Min
. Pea k

Width : Jmocthin g Width : R T Window : Expecte dRT : Us e Relativ e RT : Irtt
. Tvps : Borentio nTims : Area : I t Height : Star t Ticne : En dTime : N o IntslliOLJa n : 5 P w : 1.0 0 o r : ; eak : M

o : 0.0 0

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S 6.00e 5

*Dat a work-u p performe d byST W Pag e 1 o f 3U0011040 2 GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o fPFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

*Dat a work-u p performe d b yST W Pag e 2 o f 3 Printin g Time : 12:07:0 7 P M Printin g Date : Monday , Septembe r 13 , 201 0 Pag e 4 7 o

f 6 0GLP10-01-01 ; Interi m Repor t 0 7 Analysi s o f PFOAi n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

Printin g Time : 12:07:0 7 P M Printin g Dace : Monday , Septembe r 13 , 201 0 Pag e 4 8 o f6 0 U0011040 2

Sarrpl e Name ; -ol00708a11 TSamp* * ID : "GLPICMJI-01-07-040 ' File : " o 100708a-Wif r • Pea k Name : -PFOA_TIC
- Mass{*s) : MIS.O/SSS. l amu.413.0/168. 9 amu,4l3.0/218. 8 amu " CommenfD/y.132.Q2Y10SF 0 (d31:10 rAnnotetion : ~ Sampl e Inds>r : i n Sa&pl e Type : Unknow n N/ A 111
.

elliQua i l.D D mi n 5.3* 6 5.2* 6 5.1* 6 5.0* 6 4.9* 6 4.6*6

- 4.7e 6 4.6* 6 4.5* 6 4.4* 6 4.3« 6 4.2*6

- 4.1* 6 4.0* 6 3.9* 6 3.e* 6 3.7*6

- 3.6*6

- 3.5*6

- 3.4* 6 3.3* 6 3.2* 6 3.1* 6 3.0* 6 2.9*6

- 2.8*6

- 2.7*6

- 2.6* 6 2.5* 6 2.4* 6 2.3* 6 2.2* 6 2.1* 6 2.0* 6 1.9*6

- 1.8* 6

1.5* 6 1.4* 6 1,3* 6 1.2* 6 1.1* 6 1.0* 6 9.0* 5 8.0* 5 7.0* 5 6.0* 5 5.0* 5 4.0* 5 3.0* 5 2.0* 5 1.0* 5 0. 0 *Dat a work-u p performe d byST W Pag e 3 o f 3Documen t rrc3:fi!i;>siyse!8brit1i«ap«Bt , fo r1 4 day s fro m 09/13/201 0 Analysi s o f PFOAi n Groundwate rSample s fro m Decatur , A L June/Jul y201 0


# 3 M Enviroranenta l Laixxratory

Metho d Metho d o f Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate r

b yLC/MS/MS ; Direc t Injectio n Analysi s Metho d Number : ETS'8-044. 0 Adoptio n Date : Upo n Signin g Effectiv e Date : Q </// 7 /Q , " l

Approve d By :



### ^//^/ o • > Willia m K

. Reagen , Laborator yManage rDat e

ETS-8-044. 0 Pag e 1 of1 1 Metho d of Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 4 9 o f 6 0Documen t twx^-t^-wmatkn^m^pmtA , fo r1 4 day s fro m 09/13/201 0 Analysi s ofPFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

1 Scop e an d Applicatio n Thi s metho d i s t o b e use d t o quantif yPerfiuorobutanoi cAci d (PFBA) , Perfluoropentanoi cAci d (PFPeA) , Perfluorohexanoi cAci d (PFHA) , Perfluoroheptanoi cAci d (PFHpA) , Perfluorooctanoi cAci d (PFOA) , Perfluorononanoi cAci d (PFNA) , Perfluorodecanoi cAci d (PFDA) , Perfluoroundecanoi cAci d (PFUnA) , Perfluorododecanoi cAci d (PFDoA) , Perfluorobutanesulfonat e (PFBS) , Perfluorohexanesulfonat e (PFHS) , an d Perfluorooctanesulfonat e (PFOS ) b yHig h Perfonnance Liqui d Chromatograph ycouple d t o a tande m Mass Spectrometri cDetecto r(LC/MS/MS ) i n clea n wate rsamples

. Wate rsample s containin g heav y particulat e ma

yrequire preparatio n b

ya n alternat e metho d suc h a s ETS-8-15 4 "Determinatio n of Perfluorinate d Acids , Alcohols , Amides , an d Sulfonate s I n Wate rB ySoli d Phas e Extractio n an d Hig h Performance Liqui d Chromatography/Mas s Spectrometry"

. Thi s metho d i s considere d a performance-base d method

. Data i s considere d acceptabl e a s lon g as th e define d Q C elements are satisfied

. Sampl e collectio n i s no

t covere d unde rthi s analytica l procedure

. 2 IVIetho d Summar y Clea n aqueou s sample s are analyze d b ydirec t injectio n usin g LC/MS/MS

. Sample s containin g heav y particulat e ma

ynot b e suitabl e fo ranalysi s b ythi s method

. Sample s containin g suspende d particulat e shoul d b e centrifug e prio rt o removin g a sampl e aliquot , o rfiltered

. Thi s i s a performance-base d method

. Metho d accurac yi s determine d fo reac h sampl e set usin g multipl e laborator ycontro l spike s a

t multipl e concentrations

. Thi s metho d als o require s that th e precisio n an d accurac yfo reac h sampl e b e determine d usin g fiel d matri xspike s t o verif ythat th e metho d i s applicabl e t o eac h sampl e matrix

. Sampl e results fo rspike s outsid e o f70 % t o 130% , ma

yb e flagge d a s suc h (wit h expande d accurac

ystatements) , o rwil l no

t b e reporte d du e t o non-complian t qualit ycontro l samples

. Fortificatio n level s fo rfiel d matri xspike s an d fo rlaborator ymatri xspike s shoul d b e a t leas t 50 % o fth e endogenou s leve l an d les s tha n 1 0 time s th e endogenou s leve l t o b e use d t o determin e th e statemen t of accurac yfo ranalytica l results

. 3 Definition s 3. 1 Calibratio n Standar d Asolutio n prepare d b

yspikin g a know n volum e ofth e Wori<in g Standar d (WS ) into a predetermine d amoun t of AST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , an d analyze d accordin g t o thi s method

. Calibratio n standard s are use d t o calibrat e th e instrumen t respons e wit h respec t t o analyt e concentration

. 3. 2 Laborator yDuplicat e Sampl e (LDS , o rLa b Dup ) Alaborator

yduplicat e sampl e i s a separat e aliquot o fa sampl e take n i n th e analytica l laborator ythat i s analyze d separatel ywit h identica l procedures

. Analysi s ofLDS s compare d t o that o fth e firs t aliquot give a measur e of th e precisio n associate d wit h laborator yprocedures , bu t no

t wit h sampl e collection , preservation , o rstorag e procedures

. 3. 3 Fiel d Blan k

(FB)/Tri p Blan k AST M Typ e 1 , HPLC grad e water , o rothe rsuitabl e water , place d i n a sampl e containe ri n th e laborator y an d treate d a s a sampl e i n al l respects , includin g exposure t o samplin g sit e conditions , storage , preservatio n an d al l analytica l procedures

. Th e purpos e o fth e F B i s t o determin e i ftest substance s o r othe rinterference s ar

e presen t i n th e fiel d environment

. Thi s sampl e i s als o referre d t o as a Tri p Blank

.

ETS-8-044. 0 Pag e 2 of1 1 Metho d of Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 5 0 o f 6 0Documen t fsC.r-'i'noi-'y i niermRfpofj- ; * • 14daysfrom ^ 09/13/201 0 Analysi s o fPFOAi n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

3. 4 Fiel d Duplicat e Sampl e (FDS , Fiel d Dup ) Asampl e collecte d i n duplicat e a t th e sam e tim e fro m th e sam e locatio n a s th e sample

. Th e FD S i s handle d unde ridentica l circumstance s an d treate d exactl yth e sam e throughou t fiel d an d laborator y procedures

. Analysi s o

f th e FD S compare d t o that ofth e firs t sampl e give s a measur e ofth e precisio n associate d wit h sampl e collection , preservatio n an d storage , as wel l a s wit h laborator yprocedures

. 

### 3. 5 Fiel d Matri xSpik e (FMS ) Asampl e t o whic h know n quantitie s ofth e targe t analyte s ar e adde d t o th e sampl e bottl e i n th e laborator y befor e th e bottle s are sen t t o th e fiel d fo rcollectio n ofaqueou s samples

. Aknown , specifi cvolum e of sampl e must b e adde d t o th e sampl e containe rwithou t rinsing. Thi s ma yb e accomplishe d b

ymakin g a "fil l t o thi s level " lin e o n th e outsid e o f th e sampl e container

. Th e FM S shoul d b e spike d betwee n approximatel y50 % an d 1 0 time s th e expecte d analyt e concentratio n i n th e sample

. I f th e expecte d rang e of analyt e concentration s i s unknown , multipl e spike s a t varyin g level s ma

yb e prepare d t o increas e th e likelihoo d that a spik

e a t a n appropriat e leve l i s made

. Th e FM S i s analyze d t o ascertai n i fan ymatri x effects , interferences , o rstabilit yissue s ma

ycomplicat e th e interpretatio n ofth e sampl e analysis

. 3. 6 Tri p Blan k

Spik e (Fiel d Spik e Contro l Sample , FSCS ) A n aliquot of AST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , t o whic h know n quantitie s ofth e targe t analyte s are adde d i n th e laborator yprio rt o th e shipmen t ofth e collectio n bottles

. Th e FSC S i s extracte d an d analyze d exactl ylik e a stud ysampl e t o hel p determin e i fth e metho d i s i n contro l an d whethe ra los s of analyt e coul d b e attribute d t o holdin g time , sampl e storag e and/o rshipmen t issues

. A lo wan d hig h FSC S are appropriat e whe n expecte d sampl e concentration s are no t know n o rma

yvary . At least on e separate , un-spike d sampl e must b e take n a t th e sam e tim e an d place as eac h FMS

. 3. 7 Laborator yContro l Sampl e (LCS ) A n aliquot o

f contro l matri xt o whic h know n quantitie s ofth e target analyte s ar e adde d i n th e laborator

ya t th e tim e of sampl e extraction

. A t leas t two level s are included , on e generall ya t th e lo wen d ofth e calibratio n curve an d on e nea rth e mi d t o uppe rrang e ofth e curve . Th e LCS s ar e extracte d an d analyze d exactl ylik e a laborator

ysampl e t o determin e whethe rth e metho d i s i n control

. LCS s shoul d b e prepare d eac h da ysample s are extracted

. 3. 8 Laborator yMatri xSpik e (LMS ) Alaborator

ymatri xspik

e i s a n aliquot ofa sampl e t o whic h know n quantitie s oftarge t analyte s ar e adde d i n th e laboratory

. Th e LM S i s analyze d exactl ylik e a laborator

ysampl e t o detennin e whethe rth e sampl e matri xcontribute s bias t o th e analytica l results

. Th e endogenou s concentration s ofth e analyte s i n th e sampl e matri xmust b e determine d i n a separat e aliquot an d th e measure d value s i n th e LM S correcte d fo rthes e concentrations

. LMS s are optiona l fo ranalysi s ofaqueou s samples

. 3. 9 Laborator ySampl e Aportio n o raliquot of a sampl e receive d fro m th e fiel d fo rtesting

. 3.1 0 Limi t o f Quantitatio n (LOQ ) Th e lowe rlimi t of quantitatio n (LLOQ ) fo ra dataset i s th e lowes t concentratio n that ca n b e reliabl y quantitate d withi n th e specifie d limits o fprecisio n an d accurac ydurin g routin e operatin g conditions

. To simplif ydat a reporting , th e LLOQ i s generall yselecte d as th e lowest non-zer o standar d i n th e calibratio n curve that meets metho d criteria

. Sampl e LLOQ s are matrix-dependent

. Th e uppe rlimi t o

f quantitatio n (ULOQ ) fo ra dataset i s th e highest concentratio n that ca n b e reliabl y quantitate d withi n th e specifie d limits ofprecisio n an d accurac ydurin g routin e operatin g conditions

. Th e highest standar

d i n th e calibratio n curve that meets metho d criteri a i s define d a s th e ULOQ

.
ETS-8-044. 0 Pag e 3 o f1 1 Metho d o f Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 5 1 o f 6 0Documen t frm^io^vsBeiimmimiiim^ , fo r1 4 day s fro m 09/13 / Analysi s o fPFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

3.1 1 Metho d Blan k A n aliquot of contro l matri xthat i s treate d exactl ylik e a laborator

ysampl e includin g exposure t o al l glassware , equipment , solvents , an d reagents that ar e use d wit h othe rlaborator ysamples

. Th e metho d blan k i s use d t o determin e i f test substance s o rothe rinterference s ar e presen t i n th e laborator y environment , th e reagents , o rth e apparatus
. 3.1 2 Sampl e Asampl e i s a n aliquot remove d fro m a large rquantit yofmateria l intende d t o represen t th e origina l source material

. 3.1 3 Stoc k

Standar d Solutio n (SSS ) Aconcentrate d solutio n o f a single-analyt e prepare d i n th e laborator ywit h a n assaye d reference compound

. 3.1 4 Surrogat e Acompoun d simila ri n chemica l compositio n an d behavio rt o th e targe t analyte(s) , bu t i s no t normall y foun d i n th e sample(s)

. Asurrogat e compoun d i s typicall ya targe t analyt e wit h a t leas t on e ato m containin g a n isotopically-labele d substitution

. I fused , surrogate(s ) are adde d t o al l sample s an d qualit y contro l samples

. Surrogate(s ) are adde d t o quantitativel yevaluat e th e entire analytica l procedur e includin g sampl e collection , preparation , an d analysis

. Inclusio n ofa sun-ogat e analyt e i s a n optiona l qualit ycontro l measur

e an d i s NO

Trequired

. 

### 3.1 5 Workin g Standar d (WS ) Asolutio n of severa l analyte s prepare d i n th e laborator yfro m SSS s an d dilute d as neede d t o prepar e calibratio n standard s an d othe rrequire d analyt e solutions

. 4 Warning s an d Caution s 4. 1 Healt h an d Safet y Th e acut e an d chroni ctoxicit yof th e standard s fo rthi s metho d have no t bee n precisel ydetermined ; however , eac h shoul d b e treate d as a potentia l healt h hazard

. Th e analyst shoul d wea rgloves , a la b coat , an d safet

yglasse s t o preven t exposure t o chemical s that migh t b e present
. Th e laborator

yi s responsibl e fo rmaintainin g a saf e wori < environmen t an d a curren t awarenes s ofloca l regulation s regardin g th e handlin g of th e chemical s use d i n thi s method

. Areference fil e ofmateria l safet y dat a sheets (MSDS ) shoul d b e availabl e t o al l personne l involve d i n thes e analyses

. 4. 2 Caution s Th e analyst mus

t b e familia rwit h th e laborator yequipmen t an d potentia l hazard s including , bu t no t limite d to , th e us e of solvents , pressurize d gas an d solven t lines , hig h voltage , an d vacuu m systems
. Refe rt o th e appropriat e equipmen t procedur e o roperato rmanua l fo radditiona l infomnatio n an d cautions

. 5 Interference s Durin g sampl e preparatio n an d analysis , majo rpotentia l contaminan t source s are reagents an d glassware

. Al l material s use d i n th e analyse s shal l b e demonstrate d t o b e fre e fro m interference s unde r condition s of analysi s b

yrunnin g metho d blanks

.

ETS-8-044. 0 Pag e 4 of1 1 Metho d o f Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 5 2 o f 6 0iocumen t mayi!D®iyBSf^erii5n«6|)oS:{it , fo r1 4 day s fro m 09/13/201 0 Analysi s o f PFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

Parts an d supplie s that contai n Teflon® shoul d b e avoide d o rminimize d du e t o th e possibilit yof interference and/o rcontamination

. Thes e ma yinclude , bu t are no

t limite d to : was h bottles , Teflon ® line d caps , autovia l caps , HPLC parts , etc
. Th e us e o

f disposabl e micropipette s o rpipette s t o aliquot standar d solution s i s recommende d t o mak e calibratio n standard s an d matri xspikes

. 

### 6 Instrumentation , Supplies , an d Equipmen t 6. 1 Instrumentatio n an d Equipmen t Ahig h performance liqui d chromatograp h capabl e ofpumpin g u p t o two solvents an d equippe d wit h a variabl e volum e injecto rcapabl e of injectin g 5-10 0 |J Lconnecte d t o a tande m Mass Spectromete r (LC/MS/MS)

. I Analytica l balance capabl e of readin g t o 0.000 1 g Adevice t o collec

t ra wdat a fo rpea k

integratio n an d quantitatio n 15-m L an d 50-m L disposabl e polypropylen e centrifug e tubes

. Gas tigh t syringes , 25pL , 50pL , lOOpL , 250IJL , 500pL , lOOOpL

. 1 m L plasti cHPLC autovial

. Disposabl e pipettes , polypropylen e o rglas s a s appropriat e Centrifug e capabl e of spinnin g 15-m L an d 50-m L polypropylen e tube s a t 300 0 rpm . 

### 6. 2 Chromatographi cSyste m Guar d Column : Pris m RP , 4. 6 m m x5 0 mm , 5 p m Analytica l Column : Betasi l C I 8,4. 6 m m x100 mm , 5 p m Temperature : 10° C Mobil e Phas e (A) : 2 m M Ammoniu m Acetat e i n Wate r Mobil e Phas e (B) : Methano l Gradien t Program :

Tim e (min ) 0. 0 0. 5 11. 0 13. 5 13. 6 17. 0 % A

9 7 9 7 5 5 9 7 9 7 % B

3 3 9 5 9 5 3 3 FlowRat e

(mL/min ) 1. 0 1. 0 1. 0 1. 0 1. 0 1. 0 Injectio n Volume : 10 0 p L Quantitation : Pea k

Are a - quadrati ccurve fit , 1/ xweighted

. RunTime : ~ 17minutes

. Th e previou s informatio n i s intende d a s a guide ; alternat e condition s an d equipmen t ma yb e use d provide d tha t dat a qualityobjective s ar e met
.
ETS-8-044. 0 Pag e 5 o f1 1 Metho d o f Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 3 o f6 0

### Documen t mHtfilo^iycgsslerfiltisapaiit , for1 4 days fro m 09/13/201 0 Analysi s o fPFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0


### 6. 3 MS/M S Syste m 6.3. 1 Mode : Electrospra yNegativ e ion , MR M mode , monitorin g th e followin g transitions : Analyt e PFB A PFPeA PFH A PFHp A PFOA PFN A PFD A PFUn A PFDoA PFB S PFH S PFO S Transitio n Monitore d 213^16 9 263^21 9 313- > 26 9 an d 313- > 11 9 36 3 - ^ 319 , 36 3 ^

16 9 an d 36 3 ^

11 9 41 3 ^ 369 , 41 3 - » 21 9 an d 41 3 ^ 16 9 46 3 - > 419 , 46 3 - > 16 9 an d 46 3 - > 21 9 51 3 - » 469 , 51 3 - > 21 9 an d 51 3 ^ 26 9 56 3 - ^ 519 , 56 3 - > 26 9 an d 56 3 - > 21 9 61 3 - > 569 , 61 3 ^

16 9 an d 61 3 ^

31 9 29 9 - » 8 0 an d 29 9 - » 9 9 39 9 - ^ 8 0 an d 39 9 - > 9 9 49 9 - ^ 80 , 49 9 ^

9 9 an d 49 9 - > 13 0 Multipl e transition s fo rmonitorin g th e analyte s i s a n option , a s summin g multipl e transition s ma yprovid e quantitatio n o f isomers tha t mor e closel ymatche s NM R dat a an d ma yhav e th e adde d benefi t of increase d sensitivity

. Th e us e o fon e daughte rio n i s acceptabl e i fmetho d sensitivityi s achieved , provide d tha t retentio n tim e criteri a are me t t o assur e adequat e specificity

. Th e previou s informatio n i s intende d a s a guide , alternat e instalment s an d equipmen t ma yb e used

. 

### 7 Reagent s an d Standard s 7. 1 Chemical s Water
- Milli-Q , HPLC grade , o rothe rsuitabl yappropriat e source s Methano l - HPLC grad e Ammoniu m Acetat e -A

. C.S

. Reagen t Grad e 

### 7. 2 Standard s Perfiuorobutanoi cAci d (PFBA- C4 acid) ; Oakwoo d Products , In c Perfluoropentanoi cAci d (PFPeA- C 5 acid , als o know n as NFPA , nonafluoropentanoi cacid) ; Alfa Aesa r Perfluorohexanoi cAci d (PFHA-C 6 acid) ; Oakwoo d Products , In c Perfluoroheptanoi cAci d (PFHpA- C 7 acid , als o know n as TDHA , tridecafluoroheptanoi cacid) ; Oakwoo d Products , In c Perfluorooctanoi cAci d (PFOA- C 8 acid) ; 3 M Perfluorononanoi cAci d (PFNA-C 9 acid) ; Oakwoo d Products , In c Perfluorodecanoi cAci d (PFDA-C1 0 acid) ; Oakwoo d Products , In c Perfluoroundecanoi cAci d (PFUnA-C1 1 acid) ; Oakwoo d Products , In c Perfluorododecanoi cAci d (PFDoA-C I 2 acid) ; Oakwoo d Products , In c Perfluorobutanesulfonat e (PFB S - C4 sulfonate) ; 3 M Perfluorohexanesulfonat e (PFH S - C 6 sulfonate) ; 3 M Perfluorooctanesulfonat e (PFO S - C 8 sulfonate) ; 3 M ETS-8-044. 0 Pag e 6 of1 1 Metho d o f Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direc t Injectio n Analysi s Pag e 54 of 6 0Documen t mayib«iyB!-!n:er;m-Repor t :J^ , fo r1 4 day s fro m 09/13/201 0 Analysi s o f PFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

Th e previou s informatio n i s intende d a s a guide

. Reagent s an d standard s fro m alternat e source s ma yb e used

. 7. 3 Reagen t Preparatio n 2 m M Ammoniu m acetat e solutio n (Analysis)—Weig h 0. 3 g ofAmmoniu m acetat e an d dissolve i n 2. 0 L o freagen t wate r Note : Alternative volume s ma yb e prepare d a s lon g a s th e ratio s ofth e solven t t o solut e ratio s ar e maintained

. 7. 4 Stoc k

Standar d Solutio n (SSS ) an d Workin g Standar d Solutio n Preparatio n Th e followin g standar

d preparatio n procedur

e serve s as a n example

. Weighe d amounts an d fina l volume s ma yb e change d t o sui t th e need s of a particula rstudy

. Fo rexample , p L volume s ma yb e spike d into volumetri cflask s whe n dilutin g stoc k

solution s t o appropriat e levels

. 10 0 pg/m L targe t analyt e SSSs—Weig h ou t 1 0 m g o fanalytica l standar d (correcte d fo rpercen t sal t an d purity ) an d dilut e t o 10Om L wit h methano l o rothe rsuitabl e solvent , i n a 10Om L volumetri cflask

. Transfe rt o a 125m L LDP E bottl e o rothe rsuitabl e container

. Prepar e a separat e solutio n fo reac h analyte

. Expiratio n date s an d storag e condition s o

f stoc k solution s shoul d b e assigne d i n accordance wit h laborator ystandar d operatin g procedure

. A n exampl e of purit yan d sal t con-ectio n i s give n belowfo rPFOS

.

, . , ^ molecula rweigh t o fanio n sal t correctio n facto r= = moclecula rweigh t ofsal t

49 9 PFO S (K- ^ )sal t correctio n facto r= - ^ = 0.927 5 53 8 1 0 m g CsFiySOs'K

* wit h purit

y90 % = 8.35m g CsFiySOs " (1 0 mg*0.90*0.9275=8.3 5 mg ) 5 Mg/m L (500 0 ng/mL ) mixe d workin g standard^Ad d 0.5m L eac h ofth e 100pg/m L SSS s t o a lOm L volumetri c flask an d brin g u p t o volum e wit h solvent

. 25 0 ng/m L mixe d workin g standard—Ad d 1.25m L o fth e 5 pg/m L -mixe d wori<in g standar d solutio n t o a 25m L volumetri cflask

an d brin g u p t o volum e wit h solvent

. 12 5 ng/m L mixe d standard—^Ad d 625p L ofth e 5 pg/mL-mixe d worthin g standar d solutio n t o a 25m L volumetri c flask an d brin g u p t o volum e wit h solvent

. Storag e Conditions—Stor e al l SSS s an d worthin g standard s i n accordance wit h laborator ystandar d operatin g procedur e o ri n a refrigerato ra

t 4°±2° C fo ra maximu m perio d of6 month s fro m th e dat e o fpreparation

.

ETS-8-044. 0 Pag e 7 o f1 1 Metho d o f Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 5 of 6 0ocumen t rria fib®iyB0deriili«fip5ftiit , fo r1 4 day s fro m 09/13/20 " Analysi s o f PFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

7. 5 Calibratio n Standard s Usin g th e workin g standard s describe d above , prepare calibratio n solution s i n AST M Typ e I water , HPLC water , o r othe rsuitabl e water , usin g th e followin g tabl e as a guideline

. Note : Volume s o fwate ran d worthin g standard s ma y b e adjuste d t o meet th e dat a qualit yobjective s addresse d i n th e genera l projec t outline

. Calibratio n level s othe r tha n thos e liste d belowca n b e prepare d a s needed

.
Concentratio n o f WS , ng/m L 12 5 12 5 12 5 12 5 25 0 25 0 25 0 25 0 500 0 500 0 500 0 Volum e o fWS.fd

.

1 0 1 5 2 0 3 0 2 0 5 0 10 0 20 0 2 5 5 0 10 0 Fina l Volum e o f

Calibratio n Standar d (m L o fAST M Typ e 1 Water , o r othe rsuitabl e water )

5 0 5 0 5 0 5 0 5 0 5 0 5 0 5 0 5 0 5 0 5 0 Fina l Concentratio n o f

Calibratio n Standard , ng/m L (ppb ) i n AST M Typ e 1 Water , o rothe rsuitabl e wate r 0.02 5 0.037 5 0.05 0 0.07 5 0,10 0 0.25 0 0.50 0 1.00 2.5 0 5.0 0 10. 0 

### 8 Sampl e Handlin g 8. 1 Wate rSampl e Preparatio n Thi s metho d i s applicabl e t o clea n wate rsamples

. Sample s containin g heav yparticulat e ma

yno t b e suitabl e fo r analysi s b

ythi s method

. Sample s containin g suspende d particulat e shoul d b e centrifug e prio rt o removin g a sampl e aliquot , o rfiltered. Thoroughl ymi xsampl e befor e removin g a n aliquot an d placin g i n a labele d plasti cautovial

. Plasti ci s preferre d ove rth e us e of glas s autovials , t o preven t th e possibl yoffluorochemical stickin g t o th e glass

. Dilut e sample , i f necessary , wit h AST M Typ e I , HPLC water , o rothe rsuitabl e water
. Prepare metho d Q C sample s an d multipl e metho d blank s an d aliquot int o labele d plasti cautovials

. Prepar e a t least five metho d blanks

. 9 Sampl e Analysi s - LC/MS/M S Analyz e th e standar

d curve prio rt o eac h set ofsamples

. Th e standar d curve ma

yb e plotte d usin g a linea rfit, weighte d 1/

xo runweighted , o rb

yquadrati cfil (

y= ax ^ •< •b x-i
- c) , weighte d 1/

xo runweighted , usin g suitabl e software

. Th e calibratio n curve s ma yinclud e bu t shoul d no

t b e force d throug h zero . Th e mathematica l metho d use d t o calculat e th e calibratio n curve shoul d b e applie d consistentl ythroughou t a study

. An ychang e shoul d b e thoroughl ydocumente d i n th e ra wdata

. Hig h and/o rlo

wpoints ma

yb e exclude d fro m th e calibratio n curve s t o provid e a bette rfit ove rth e rang e appropriat e t o th e dat a o rbecaus e theydi d no t meet th e pre-detemnine d acceptance criteria

. Low-leve l curve points shoul d als o b e exclude d i f thei rare a counts ar e no t a t least twic e that ofth e metho d and/o rsolven t blanks

. Th e coefficien t of detenninatio n (r^ ) valu e fo rth e calibratio n curve must b e greate rtha n o requa l t o 0.990

. Eac h poin t i n th e curve mus

t b e withi n ±25 % ofth e theoretica l concentratio n wit h th e exceptio n ofth e LLOQ , whic h ma y ETS-8-044. 0 Pag e 8 o f1 1 Metho d o f Analysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 5 6 o f 6 0Documen t LC.P Koi-o i nterm-Repot-jV , fo r1 4 day s fro m 09/13/20 ' Analysi s ofPFOAi n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

b e withi n ±30%

. Justificatio n fo rexclusio n ofcalibratio n curve points wil l b e note d i n th e ra wdata

. Aminimu m of6 points wil l b e use d t o constaict th e calibratio n curve . I f th e calibratio n curve doe s no t meet acceptance criteria , perfor m routin e maintenance o rprepare a ne wstandar d curve (i f necessary

) an d reanalyze

. Continuin g calibratio n verification s (CCV) are analyze d t o verif yth e accurac

yofth e calibratio n curve . Analyz e a mid-rang e calibratio n standard , on e o fth e sam e standard s use d t o construc t th e calibratio n curve , a

t a minimu m afte rever ytent h sample , no

t includin g solven t blanks , wit h a minimu m ofon e pe rsampl e set
. Calibratio n verificatio n injection s must b e withi n ±25 % t o b e considere d acceptable

. Th e calibratio n curve an d th e las t passin g CC V wil l the n bracket acceptabl e samples

. Multipl e CCV level s ma yb e used

. Sample s containin g analyte s that are quantitate d above th e concentratio n ofth e highest standar d i n th e curve shoul d b e furthe rdilute d an d reanalyzed

. 1 0 Qualit yContro l
10. 1 Dat a Qualit yObjective s Thi s metho d an d require d qualit ycontro l sample s i s designe d t o generat e dat a accurat e t o ±30 % wit h a targete d LO Q o f 0.02 5 ng/mL

. An ydeviation s fro m th e qualit ycontro l measure s spelle d ou t belo wwil l b e documente d i n th e ra wdata an d footnote d i n th e final report
. 

### 10. 2 Metho d Blank s Metho d blank

s must b e prepare d wit h eac h analysi s batch

. At least five metho d blank s must b e prepared

. Metho d blank

s ma yb e injecte d multipl e times , bu t n o mor e tha n 3 injection s shoul d b e remove d fro m a singl e metho d blank

. At a minimum , metho d blank s ar e analyze d prio rt o instrumen t calibration , prio rt o th e analysi s o f CCV samples , an d a

t th e en d of th e analytica l run . Th e mea n are a coun t fo reac h analyt e i n th e metho d blank s must b e les s tha n 50 % ofth e are a coun t ofth e LOQ standard

. Th e standar

d deviatio n of th e are a count s ofthes e metho d blank s shoul d b e calculate d an d reported

. I f th e mea n are a counts of th e metho d blank s excee d 50 % ofth e LOQ standard , the n th e LOQ mus t b e raise d t o th e first standar

d leve l i n th e curve that meets criteria , o ralternatively , th e metho d blank s mus t b e evaluate d statisticall yt o detennin e outliers , o rtechnica l justificatio n t o eliminat e on e o rmor e results shoul d b e made

. 

### 10. 3 Sampl e Replicate s Sample s duplicate s are collecte d i n th e field. Th e relative percen t difference , RPD , shoul d b e reported

. RP D results greate rtha n 20 % wil l b e flagged i n th e report , bu t wil l no t b e exclude d fro m reporting

. Th e requiremen t fo r replicate s exclude s field blanks

. 10. 4 Surrogat e Spike s Surrogat e spike s are no

t require d bu t ma

yb e use d o n projec

t specifi crequirements

. 

### 10. 5 La b Contro l Sampl e Triplicat e la b contro l spike s a t a minimu m o

ftwo differen t concentration s are t o b e prepare d wit h eac h preparatio n batch

. Lo wla b contro l spike s shoul d b e prepare d a t concentration s i n th e rang e offive t o te n time s highe rtha n th e targete d LOQ an d hig h la b contro l spike s shoul d b e prepare d a t concentration s nea rth e mid-poin t ofth e curve . Th e relative standar

d deviatio n of th e contro l spike s evaluate d independentl ya t eac h concentratio n leve l mus t b e les s tha n o requa l t o 20 % an d th e averag e recover ymust b e 80-120%

. I fth e above criteri a are no t met , th e entir

e set o f sample s shoul d b e re-injecte d o rre-prepare d a s appropriate

.

ETS-8-044. 0 Pag e 9 o f1 1 Metho d o f Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 7 of6 0Documen t msfk)mmeiktii\tmpm^ , for1 4 day s fro m 09/13/201 0 Analysi s o fPFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

10. 6 Fiel d Matri xSpike s / La b Matri xSpike s Recoverie s of field matri xspike s an d laborator ymatri xspike s ar

e anticipate d t o b e betwee n 70 % an d 130 % o fth e fortifie d levels

. Sampl e results fo rspike s outsid e o f70 % t o 130% , ma

yb e flagged as suc h (wit h expande d accurac ystatements) , o rwil l no

t b e reporte d du e t o non-complian t qualit ycontro l samples

. Th e targete d fortificatio n level s shoul d b e a t leas t 50 % ofth e endogenou s leve l an d les s tha n 1 0 time s th e endogenou s leve l t o b e use d withou t justificatio n t o detennin e th e statemen t ofaccurac yfo ranalytica l results

. Th e averag e of th e sampl e an d th e field duplicat e shoul d b e use d t o calculat e th e recovery . 1 1 Dat a Analysi s an d Calculation s Us e th e followin g equatio n t o calculat e th e amoun t ofanalyt e foun d (i n ng/mL , base d o n pea k area) usin g th e standar d curve (linea rregressio n parameters ) generate d b ya n appropriat e softwar

e program :

. , ^ , . , , , , (Pea k Area-Intercept ) ^

_ Analyt e foun d (ng/mL ) = - ^ ^-^

xD F
D F = facto rb

ywhic h th e final volum e wa s diluted , i fnecessary . Fo rsample s fortifie d wit h know n amounts ofanalyt e prio rt o extraction , us e th e followin g equatio n t o calculat e th e percen t recovery .

_Tota l analyt e foun d (ng/mL ) - Averag e analyt e foun d i n sampl e (ng/mL ) Analyt e adde d (ng/mL )
1 2 Metho d Performanc e An ymetho d perfonnanc e parameter s that are no

t achieve d must b e considere d i n th e evaluatio n o fth e data

. Nonconfonnance t o an yspecifie d parameter s must b e describe d an d discusse d i fth e Technica l Manage r(non
GL P study) o rStud yDirecto r(GL P study) choose s t o repor t th e data

. I f criteri a liste d i n thi s metho d performance sectio n are no t met , maintenance ma

yb e performe d o n th e syste m an d sample s reanalyzed , o rothe raction s take n as appropriate

. Documen t al l action s i n th e ra wdata

. I f dat a are t o b e reporte d whe n perfonnance criteri a hav e no t bee n met , th e dat a mus t b e footnote d o n table s an d discusse d i n th e tex

t o f th e report
. 12. 1 Syste m Suitabilit y Syste m Suitabilit

ystandard s are no

t a require d componen t ofthi s method

. I frequire d b yprotoco l o rb

yth e technica l manager , a minimu m of thre e syste m suitabilit ysample s ar

e injecte d a

t th e beginnin g ofeac h analytica l ru n prio rt o th e calibratio n curve . Typicall ythes e sample s are a t a concentratio n nea rth e mi d leve l o fth e calibratio n curve an d are repeate d injection s fro m on e autosample rvial

. Th e syste m suitabilit yinjection s mus

t have are a count s wit h a n RS D of S5% an d a retentio n tim e RS D o f^2 % t o b e compliant

. 12. 2 Quantitatio n Calibratio n Curve : Th e coefficien t of detenninatio n (r^ ) valu e fo rth e calibratio n curve mus t b e greate rtha n o r equa l t o 0.990

. Eac h poin t i n th e curve must b e withi n ±25 % ofth e theoretica l concentratio n wit h th e exceptio n of th e LLOQ , whic h ma

yb e withi n ±30%

. CCV Performance : Th e calibratio n standard s that are intersperse d throughou t th e analytica l sequence ar e evaluate d a s continuin g calibratio n verification s i n additio n t o bein g par t ofth e calibratio n curve . Th e accurac yo f eac h curve poin t mus

t b e withi n 25 % ofth e theoretica l valu e (withi n 30 % fo rlowes t curve point)

. Sample s that ar e brackete d b

yCCVs no

t meetin g thes e criteri a mus t b e reanalyzed

. ETS-8-044. 0 Pag e 1 0 of1 1 Metho d of Analysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 5 8 o f 6 03ocum € ,G-Picoi-o-'f!n!ermR«poto 7 : . . 1 4 day s fro m Analysi s o fPFOAi n Groundwate rSample s fro m Decatur , A L June/Jul y201 0

Demonstratio n o f Specificity : Specificit yi s demonstrate d b

ychromatographi cretentio n tim e (withi n 4 % of standard ) an d th e mas s spectra l respons e o funiqu e ions

. 

### 12. 3 Sensitivit y Th e targete d limi t of quantitatio n fo ral l analyte s i s 0.02 5 ng/mL

. Th e LOQ fo ran yspecifi canalyt e ma yvar y dependin g o n th e evaluatio n o f appropriat e blank

s an d th e accurac

yofth e low-leve l calibratio n curve points

. Refe r t o Sectio n 1 0 fo radditiona l details

. 12. 4 Accurac y Thi s metho d an d require d qualit ycontro l sample s ar

e designe d t o generat e data that ar e accurat e t o +/-30%

. Sectio n 1 0 contain s additiona l informatio n regardin g th e require d accurac yo flaborator

ycontro l spikes , field matri x spike s an d laborator

ymatri xspikes

. 12. 5 Precisio n Sample s shoul d b e collecte d i n duplicat e i n th e field. Th e relative percen t difference , RPD , shoul d b e reported

. RP D results greate rtha n 20 % wil l b e flagged i n th e report , bu t wil l no t b e exclude d fro m reporting

. Th e requiremen t fo rreplicate s exclude s field blank s o rrinse blanks

. Sectio n 1 0 contain s additiona l infomnatio n regardin g th e require d precisio n oflaborator ycontro l spikes

. 

### 1 3 Pollutio n Preventio n an d Wast e Managemen t Wast e generate d whe n perfomnin g thi s metho d wil l b e dispose d o fappropriately

. Th e origina l sample s wil l b e archive d a

t th e 3 M Environmenta l Laborator yi n accordance wit h interna l procedures

. 1 4 Record s Eac h data packag e generate d fo ra stud ymus t includ e al l supportin g infomnatio n fo rreconstructio n o f th e data

. Infomnatio n fo rth e dat a packag e must include , bu t i s no t limite d t o th e followin g items : stud yo rprojec t number , sampl e an d standar

d pre p sheets/records , instrumen t ru n lo g (instmmen t batc h records , instrumen t acquisitio n method , summar

ypages) , instrumen t results files, chromatograms , calibratio n curves , an d dat a calculations

. 1 5 Affecte d Document s None

. 1 6 Revision s Revisio n Numbe rSummar yofChange s

ETS-8-044. 0 Pag e 1 1 of1 1 Metho d of Analysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 5 9 o f6 03 M Confidentia l GLP10-01-01 ; interi m Repor t 0 7 Analysi s o fPFO Ai n Groundwate rSample s fro m Decatur , A L June/Jul y201 0 

## RECOR D O F DEVIATION/NONCONFORMANC E

/

. Identificatio n stud y/ Project No

. GLP10-01-01-0 7 Deviatio n typ e 5 (Chec k one ) D I Date(s ) of Occurrence :

i o100708aan d m100812 a SO P D Equipmen t Procedur e Protoco l 0 GP O Documen t Number : ETS-8-044. 0 0 D Metho d Other : //

. Descriptio n (attac h extr a page s a s needed ) Metho d Requirements : 1

. LC S averag e recover yo f 100 % ±20%

. 2

. CC V recover

yo f 100 % ±25 % analyze d ever ytent h sample

. 3

. FM S recover

yo f 100 % ±30%

. Actua l procedure/process : (1 ) LC S averag e recover yfo rbranche d PFOAwa s >120%

. I t appears tha t ther e i s a n analytica l bia s whe n quantitatin g branche d isomers o fPFOAagains t a calibratio n curv e prepare d fro m linea rPFOA(o100708 a an d m l 00812a)

. (2 ) Thre e o f th e endin g CCV s analyze d durin g th e o100708 a ru n ha d recoverie s rangin g fro m 71.0 % t o 74.1%

. (0100708a)

. (3 ) Tw o locations , 137 L an d 134 S ha d on e FM S recover ya t >130 % (o100708a)

. ///

. Action s Take n (suet ) a s amendmen t issued , SO P revision , etc. ) Correctiv e Actio n ( D Ye s 0 No ) Reference : Acceptabilit yo f th e nonconformin g work : 1 ) Th e linea r+ branche d PFOALC S whe n quantitate d agains t a calibratio n curv e prepare d fro m linea rPFOAhav e bee n quantitatin g aroun d 15-30 % higher

. B yquantitatin g th e linea ran d branche d isomers o f PFOAseparately , agains t a linea rPFOAcurve , an d summin g th e resultin g concentrations , appears t o hel p reduc e th e recover yo fth e linea r+ branche d PFOA by5-15%

. Th e metho d analytica l uncertaintywa s determine d base d o n th e highes t averag e recover yfo rth e linea r+ branche d PFOALC S (141%)

. 2 ) Twenty-on e CCV s wer e analyze d durin g th e cours e o fth e ru n (o100708a ) wit h th e thre e endin g CCV s jus t outsid e th e acceptanc e criteria

. Reporte d sampl e result s brackete d b y thes e endin g CCV s wil l b e note d i n th e final report
. 3 ) Th e tw o location s wit h FM S recoverie s outsid e metho d acceptanc e criteri a wil l b e footnote d i n th e final report
. _ Actions : D Haltin g o f Wor k D Clien t Notificatio n D Wor k Recal l IZ i Other : Deviation s wil l b e note d i n fina l report
. D Withholdin g ofRepor t Projec t Lead/PA I Approval : Sjusa n Wol f Stu^ yDTrectorTi f GCPF " ~^ ^ Date ; 

# Ma / / o Date : m ' Sponso rApprova l (fo rGLFnprotoco l deviations) : N A Technica l Reviewe r(optional) : N A Date : N A Laborator yDepartmen t Manage rApproval : Date : IV

. Authorizatio n t o Resum e Wor k Wfier e tialtin g o fwor k occurred , resumptio n o f wor k mus t firs t b e approve d b yLaborator yManagemen t LaboratoryDepartmen t ManagerApproval : NADate : N A Deviatio n No

. (assigne d b yStud yDirecto ro rTea m Leade ra t th e en d o fstud yo rproject )
Attachmen t AETS-4-008. 7 Pag e 1 o f1

Documentatio n o f Deviation s an d Contro l o fNonconformin g Testinc , ^^^ ^ ^ ° ° ' ^ °